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Chemical Structure| 62-54-4
Chemical Structure| 62-54-4
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Product Details of [ 62-54-4 ]

CAS No. :62-54-4 MDL No. :MFCD00150019
Formula : C4H6CaO4 Boiling Point : -
Linear Structure Formula :- InChI Key :VSGNNIFQASZAOI-UHFFFAOYSA-L
M.W : 158.17 Pubchem ID :6116
Synonyms :
Chemical Name :Calcium acetate

Safety of [ 62-54-4 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 62-54-4 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 62-54-4 ]

[ 62-54-4 ] Synthesis Path-Downstream   1~109

  • 1
  • [ 62-54-4 ]
  • [ 5743-36-2 ]
  • [ 589-38-8 ]
  • 2
  • [ 62-54-4 ]
  • [ 5743-36-2 ]
  • [ 107-87-9 ]
  • 3
  • [ 62-54-4 ]
  • [ 108-24-7 ]
YieldReaction ConditionsOperation in experiment
With Benzotrichlorid at 170 - 180℃;
With Benzotrichlorid at 230 - 240℃; im Rohr;
With acetic acid; Benzotrichlorid unter Rueckfluss;
With acetic anhydride; Benzotrichlorid unter Rueckfluss;
With Benzotrichlorid; toluene unter Rueckfluss;
With sulfuryl dichloride; sulfur trioxide; acetic anhydride
With chlorosulfonic acid
With chlorosulfonic acid; sulfuryl dichloride
With chlorosulfonic acid; pyrosulfuryl chloride
With disulfur dichloride; chlorosulfonic acid
With tetrachloromethane; phosgene; sulfur trioxide Reagens 4: Schwefelsaeurechlorid;
With chlorosulfonic acid; sulfur trioxide

Reference: [1]Current Patent Assignee: WACKER CHEMIE AG - DE368340, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251]
[2]Current Patent Assignee: WACKER CHEMIE AG - DE368340, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251]
[3]Current Patent Assignee: WACKER CHEMIE AG - DE368340, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251]
[4]Current Patent Assignee: WACKER CHEMIE AG - DE368340, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251]
[5]Current Patent Assignee: WACKER CHEMIE AG - DE368340, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 251]
[6]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE358774, 1922, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 13, p. 1116][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 13, p. 1116]
[7]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE372716, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253]
[8]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE372716, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253]
[9]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE372716, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253]
[10]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE372716, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253]
[11]Current Patent Assignee: Beatty - DE290702, 1800, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 12, p. 79][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 12, p. 79]
[12]Current Patent Assignee: A. MENARINI - INDUSTRIE FARMACEUTICHE RIUNITE - S.R.L. - DE372716, 1923, C [Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253][Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 253]
  • 5
  • [ 108-24-7 ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
98.8% With water monomer; calcium(II) oxide at 65 - 70℃; for 6h; 6 Conversion of Acetic Anhydride to Calcium Acetate To a three-necked round bottom flask placed in a heating mantle and equipped with a mechanical stirrer, temperature-measuring thermocouple, and pressure-equalizing dropping funnel, was added 15 g (0.25 mole) of lime (95%; Specialty Minerals, Inc), followed by enough city water (159.9 g) to make a mixable slurry. The temperature of the slurry did not exceed 65° C. To this stirred slurry was dropwise added 24.9 g (0.24 mole) of acetic anhydride (99%; Fisher) over a period of 2 hr. After this addition was complete, the reaction solution was kept at 70° C. for 4 hr. After this time, the pH of the final reaction solution was 12 and enough acetic acid was added to reduce the pH to 7.0. Analysis of the reaction solution by HPLC showed it to be an aqueous solution of essentially pure calcium acetate. The water was removed by evaporation to give 38.1 g of dry calcium acetate (98.8% yield) as an essentially pure white solid.
With anhydrous calcium nitrate
  • 7
  • [ 62-54-4 ]
  • lauracidic calcium [ No CAS ]
  • [ 593-08-8 ]
  • 8
  • [ 62-54-4 ]
  • α-methyl-hydrocinnamate of calcium [ No CAS ]
  • [ 21869-55-6 ]
  • 9
  • [ 62-54-4 ]
  • [ 134523-00-5 ]
  • [ 134523-03-8 ]
YieldReaction ConditionsOperation in experiment
84.35% EXAMPLE 3 Preparation of <strong>[134523-00-5]Atorvastatin</strong> Calcium Crystalline Form VI 360 liters of acetonitrile and 24 kg of <strong>[134523-00-5]atorvastatin</strong> was taken into a reactor and subjected to heating to 44 C. for 1 hour. 73 liters of 10% aqueous calcium acetate solution was added to the reaction mass and maintained for 1 hour, 15 minutes. 4.5 liters of 10% aqueous sodium hydroxide was added to the above reaction mass and subjected to heating to reflux at 70 C. for 1 hour. The reaction mass was filtered and the solid washed with 45 liters of acetonitrile. 9 liters of 10% sodium hydroxide was added to the above solid and subjected to heating to reflux at 70 C. for a period of about 8 hours. The reaction mass was cooled to 30 C. for a period of about 1.5 hours and centrifuged followed by washing with 112.5 liters of water. The obtained solid material was spin dried for a period of about 2 hours and kept for aerial drying for 30 minutes. The obtained solid material was dried at 55 C., cooled and the solid was thoroughly mixed. Finally the obtained solid material was subjected to rotatory cone vacuum drying to afford 35.8 kg (84.35%) of crystalline Form VI of <strong>[134523-00-5]atorvastatin</strong> calcium.
  • 10
  • [ 62-54-4 ]
  • mupirocin [ No CAS ]
  • calcium mupirocin [ No CAS ]
YieldReaction ConditionsOperation in experiment
87% With ammonium sulfate; sodium hydroxide In water Tris-buffer; 2.B B. A filtrate obtained as in Example 1 (293 ml, 1.5 g mupirocin), was added (NH4J2SO4 (19 g). The pH was adjusted to pH 7.5 by addition of 1M NaOH. The polystyrene divinylbenzene adsorbent XAD1600 (Rohm & Haas) was packed into a chromatography column (22 ml) and the prepared mupirocin solution (in the form of pseudomonate solution) was added to the column (1 ml/min). The column was washed with a 0.1 M Tris-buffer containing 0.5M (NH4)2SO4, pH 7.5 (110 ml). A 0.1 M calcium acetate solution was subsequently added to the column (66 ml), followed by water (66 ml). Mupirocin calcium was eluted from the column with 80% methanol. 1.3 g mupirocin calcium was recovered in the elution pool (55 ml, 87% yield).
70% With ammonium sulfate; sodium hydroxide In water Tris-buffer; 2.A; 2.C Example 2; Adsorption of pseudomonic acid to a solid support and conversion to mupirocin calciumA. A filtrate obtained as in Example 1 (363 ml, 1.3 g mupirocin) was added (NH4)2SO4 (24 g). The pH was adjusted to pH 7.5 by addition of 1 M NaOH. The acrylic adsorbent XAD7HP (Rohm & Haas) was packed into a chromatography column (24 ml) and the prepared mupirocin solution (in the form of pseudomonate solution) was added to the column (1 ml/min). The column was washed with 0.1 M Tris-buffer containing 0.5M (NH4J2SO4, pH 7.5 (120 ml). A 0.1 M calcium acetate solution was then added to the column (72 ml), followed by water (48 ml). Mupirocin calcium was eluted from the column with 80% methanol. 0.9 g mupirocin calcium was recovered in the elution pool (60 ml, 70% yield). C. A filtrate obtained as in Example 1 (1035 ml, 5.8 g mupirocin), was added (NH4J2SO4 (68 g). The pH was adjusted to pH 7.5 by addition of 1 M NaOH. The acrylic adsorbent XAD7HP (Rohm & Haas) was packed into a chromatography column (191 ml_) and the prepared mupirocin solution (in the form of pseudomonate solution) was added to the column (1.9 ml/min). The column was washed with 0.1 M Tris-buffer containing 0.5M (NH4)2SO4, pH 7.5 (958 ml). A 0.1 M calcium acetate solution was added to the column (575 ml), followed by water (573 ml). Mupirocin calcium was eluted from the column with 60% methanol. 5.0 g mupirocin calcium was recovered in the elution pool (216 ml, 83% yield).A fraction of the elution pool (54 ml, 1.2 g mupirocin calcium) was evaporated (90 mbar, 500C). The resulting methanol free solution (15 ml) was allowed to crystallize with stirring at room temperature. After approximately 20 hr the crystalline material was filtered off and the resulting filter cake was washed with water (10 ml) and dried in a vacuum tray dryer (<50 mbar, 400C). 1.1 g product was recovered with a specific activity of 91.4% ('as is').
  • 11
  • [ 15572-79-9 ]
  • [ 62-54-4 ]
  • [ 17598-82-2 ]
YieldReaction ConditionsOperation in experiment
44% With calcium hydroxide In H2; CO2; water 6 EXAMPLE 6, Isomerization of L-Galactose, Calcium Acetate Catalyst EXAMPLE 6 Isomerization of L-Galactose, Calcium Acetate Catalyst To a 25 ml Erlenmeyer flask, equipped with a magnetic stirrer, was added 0.5 g L-galactose, 5 ml water, 0.2 g calcium hydroxide, and 22 mg calcium acetate. The mixture was stirred. After 2 hours, the solution was filtered to collect the calcium hydroxide-L-tagatose complex that had formed. The sticky complex was resuspended in 5 ML of H2, and CO2was bubbled through the slurry until the PH was below 7. The solution, after filtering off the calcium carbonate, was deionized as in Exampie 1 and concentrated in vacuo to a syrup which, after seeding with a few L-tagatose crystals, provided 0.22 g of pure L - tagatose, a 44 % yield.
44% With calcium hydroxide In water 6 Isomerization of L-Galactose, Calcium Acetate Catalyst EXAMPLE 6 Isomerization of L-Galactose, Calcium Acetate Catalyst To a 25 ml Erlenmeyer flask, equipped with a magnetic stirrer, was added 0.5 g L-galactose, 5 ml water, 0.2 g calcium hydroxide, and 22 mg calcium acetate. The mixture was stirred. After 2 hours, the solution was filtered to collect the calcium hydroxide-L-tagatose complex that had formed. The sticky complex was resuspended in 5 mL of H2 O, and CO2 was bubbled through the slurry until the pH was below 7. The solution, after filtering off the calcium carbonate, was deionized as in Example 1 and concentrated in vacuo to a syrup which, after seeding with a few L-tagatose crystals, provided 0.22 of pure L-tagatose, a 44% yield.
  • 12
  • [ 7784-27-2 ]
  • [ 62-54-4 ]
  • mayenite [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: aluminium trinitrate; calcium acetate With citric acid In water at 20℃; Stage #2: at 1350℃; for 5h; 1 Example 1 Preparation of the Catalyst Consisting of Pure Mayenite (Already Described in Example 1 of Patent Application IT-M199A002616). [0045] A synthesis method in homogeneous phase was used. [0046] This method comprises the use of citric acid or polyfunctional hydroxy-acids with the function of complexing metal salts in aqueous solution. After dehydrating the aqueous solution, an amorphous precursor solid is obtained, which, after high temperature thermal treatment, produces the desired product. [0047] The main advantages of this technique are: [0048] homogeneous mixing on an atomic level [0049] good stoichiometric control [0050] production of mixed oxides using commercial chemical products [0051] short process times. [0052] A solution of aluminum nitrate, 378.2 g of Al(NO3)3.9H2O (1.008 moles in 470 g of water was first added to a solution of calcium acetate, obtained by dissolving 152.2 g of (CH3COO)2Ca.H2O (0.864 moles) at room temperature in 450 g of H2O, followed by a solution of citric acid: 393.1 g (1.872 moles) in 375 g of water. The homogeneous solution obtained was dried by means of a spray-dryer. The desired product 12CaO.7Al2O3 (Mayenite) was obtained in pure form after calcination at 1350° C. for 5 h. [0053] In order to obtain a catalyst formed by pelletizing, a lubricating agent was added (2 wt % of stearic acid); after pelletizing the catalyst was subjected to a further calcination step. [0054] The composition of the catalyst obtained was verified by means of X-ray diffractometry which revealed the presence of the sole pure 12CaO.7Al2O3 phase. [0055] (See Table I and FIG. 1 mentioned above).
  • 13
  • [ 62-54-4 ]
  • [ 24634-61-5 ]
  • calcium acetate sorbate [ No CAS ]
YieldReaction ConditionsOperation in experiment
73% In water at 25℃; for 0.0833333h; 1 EXAMPLE 1; Preparation of a Calcium Double Salt of Sorbic Acid and Acetic Acid 158 g (1 mol) of calcium acetate are dissolved in 420 ml of water. To this solution are added, at 25° C., a solution of 56 g (0.37 mol) of potassium sorbate in 60 ml of water. During the addition a precipitate forms immediately which is filtered off after 5 min. The precipitate is dried to constant weight at 100 mbar and 50° C. 88% pure calcium acetate sorbate is obtained as a white powder in 73% yield.
  • 14
  • [ 13477-34-4 ]
  • [ 6303-21-5 ]
  • [ 62-54-4 ]
  • tricalcium diphosphate [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium(II) nitrate; hypophosphorous acid; calcium acetate In water at 20 - 25℃; for 0.05h; Stage #2: at 500℃; for 1h; 3 An aqueous solution of 8.51 g 50 wt % H3PO2 was combined with 8.00 g of 25.0 wt % aqueous solution of calcium acetate monohydrate, Ca(O2CCH3)2.H2O (ACS reagent, Aldrich Chemical Co., Inc. No.40,285-0, CAS 5743-26-0), equivalent to 5.69 wt % Ca, to give a clear, colorless solution contained in a 250 ml Pyrex beaker. To this solution was added 20.17 g Ca(NO3)24.H2O salt. The molar ratio of Ca/phosphate in this mixture was 3/2 and the equivalent solids level [as Ca3(PO4)2] was 27.3 wt %. Endothermic dissolution of the calcium nitrate tetrahydrate salt proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction which proceeded as described in Example 1. After approximately three minutes, the reaction was essentially complete leaving a moist, white, crumbly solid which was hot to the touch and which smelled of acetic acid. After cooling to room temperature, the solid was stored in a polyethylene vial. [0199] Heat treatment and X-ray diffraction analysis of this solid were conducted as described in Example 1. Following heat treatment in air at 500° C. for either 0.5 or 1 hour, XRD indicated the solid to be composed of whitlockite as the primary phase along with hydroxyapatite as the secondary phase. XRD results indicate that the relative ratio of the two calcium phosphate phases was dependent on the duration of the heat treatment and the presence of the acetate anion, but no attempts were made to quantify the dependence. [M00001] [0200] Comparing the XRD spectra from these results in Example 3 with XRD spectra from Example 1 shows the difference in the amount of HAp-Ca5(PO4)3-x(CO3)x(OH) phase present for each minor phase. The samples in Example 1 exhibited no acetate whereas the samples in Example 3 showed acetate present. This is indicative of the counteranion effect on crystal formation. [0201] Fourier Transform Infrared (FTIR) spectra were obtained using a Nicolet model 5DXC instrument (Nicolet Instrument Co., 5225 Verona Rd. Madison, Wis. 53744) run in the diffuse reflectance mode over the range of 400 to 4000 cm-1. The presence of the carbonated form of HAp is confirmed by the FTIR spectra, which indicated the presence of peaks characteristic of [PO4]-3 (580-600, 950-1250 cm-1) and of [CO3]-2 (880, 1400, & 1450 cm-1). The PO stretch, indicated by the strong peak at 1150-1250 cm-1, suggests a structural perturbation of hydroxyapatite by the carbonate ion.
  • 15
  • [ 62-54-4 ]
  • [ 752190-89-9 ]
  • [ 64-19-7 ]
YieldReaction ConditionsOperation in experiment
With sulfur dioxide; water at 20 - 60℃; 2 EXAMPLE 2 Recovery of Acetic Acid with Sulfur Dioxide [0039] Materials and Methods [0040] Materials [0041] Calcium acetate (99.8%) and sulfur dioxide (anhydrous, 99.98%) used in this research was purchased from Fisher Scientific International Inc. and Matheson Tri-Gas Inc. (Montgomeryville, Pa.), respectively. [0042] Apparatus and Operational Procedures [0043] A 500 mL reactor (Chemglass, Inc., Vineland, N.J.) was used to conduct all experiments. Temperature control was realized using a Neslab RTE-111 bath/circulator, which circulated a low-temperature oil (Ace Glass, Inc., Vineland, N.J.) through the jacket of the reactor. To avoid water loss through evaporation, the outlet gas from the reactor passed through a condenser that was maintained at approximately 3° C. by a heated/refrigerated Cole Parmer Polystat 6-liter circulator unit. The inlet and outlet concentrations of SO2 in the gas stream were monitored using a California Analytical model ZRF NDIR gas analyzer (manufactured by Fuji Electric Company, Saddle Brook, N.J.). The gas analyzer reads 0 to 10 v % SO2 by 0.01% and has a repeatability of +/-0.5% of full scale. The SO2 readings of the gas analyzer were recorded with a computer-based data collection system every 10 seconds for further analysis. During the experiments, the reaction mixture in the reactor was stirred at 60 rpm for all trials by an adjustable overhead stirrer connected to a Teflon mixer. Mass measurements of the calcium acetate and water were made on a Mettler model PM4000 balance with a linearity of +/-0.02 g. The flow rates of gases were controlled with flow meters. Reaction temperature was measured with a non-mercury glass thermometer inserted into the reaction mixture. [0044] The first step of the reaction was to add 40.0 g Ca(CH3COO)2.H2O into a reactor filled with 245.5 g deionized water and then to stir the mixture continuously at 60 rpm for 30 minutes to completely dissolve all of the added calcium acetate. Since the final concentration of acetic acid generated for all tests was set to be 1.667 M, the quantities of calcium acetate and water added in each test were the same. N2 and SO2 were then sparged into the reactor solution through an 8 mm glass tube to start the reaction. The SO2 gas analyzer was calibrated before and after each test run. The calibrations were performed with known concentrations of standard gases supplied by BOC Gases, Des Moines, Iowa. Each experiment was ended when the outlet concentration of SO2 was the same as the inlet concentration. [0045] Variables used in this research include reaction temperature and concentration of SO2 in the gas stream, with a total flow rate of 3447.0 mL/min. The reaction temperature varied from 20 to 60° C., with an interval of 10° C. The concentration of SO2 in the gas mixture varied from 3.0 to 9.0 v %, with an interval of 1.5 v %. [0046] Analysis of Acetic Acid with HPLC [0047] The acetic acid produced from R1 was analyzed with a Waters 501 high-performance liquid chromatograph (HPLC). The organic acid analysis column used was provided by Alltech Prevail (Alltech Associates, Inc). The material used in mobile phase was a degassed KH2PO4 solution (0.005 M). The HPLC operation parameters during the measurements of acetic acid include: 1) 192 nm of UV light, 2) a column pressure of 900 psi, and 3) a mobile phase flow rate of 0.8 mL/min. [0048] Results and Discussion [0049] Once sulfur dioxide was sparged into the calcium acetate solution, it underwent a series of steps before reacting with the calcium acetate, including gas phase diffusion, mass transfer at the gas-liquid interface, hydrolysis and ionization of the dissolved SO2, and aqueous diffusion and reaction between the calcium acetate and sulfurous acid. The solubility of SO2 in 100.0 g water is 10.6 g at a temperature of 20° C. and 3.2 g at 60° C., which means that the quantity of SO2 dissolved in water is considerable given enough time. However, the rate of SO2 dissolved into water was so slow that the SO2 concentration difference in the inlet and outlet stream was negligible when only water existing in the reaction vessel. After addition of calcium acetate in the water, the experiment showed that the SO2 concentrations in the outlet stream remained at zero throughout the process. This suggested that the solution's capacity for absorption of SO2 was greatly increased by the dissolution of calcium acetate. When SO2 was dissolved into the solution containing calcium acetate, it reacted to yield HSO3- and SO32-, thereby lowering the dissolved SO2 concentration and allowing more total SO2 from the gas phase to be dissolved. [0050] The solubility of Ca(CH3COO)2 in 100.0 g of water is 37.4 g at a temperature of 0° C. and 29.7 g at 1001C. Under experimental conditions, the added calcium acetate was completely dissolved. The produced calcium sulfite, however, had a very low solubility in water: 0.0043 g at 18° C. and 0.0011 g at 100° C. in 100.0 g water. When SO2 was sparged into the solution, it dissolved in the water and reacted with calcium acetate to produce calcium sulfite precipitate and acetic acid. Calcium sulfite was separated from the liquid with a simple filtration process. [0051] In the experimental design, the assumption was made that the reaction endpoint would be reached when concentrations of SO2 in the inlet and outlet mixture gases were identical. At the beginning of the reaction, the outlet gas from the reactor was nondetectable, indicating that the SO2 in the gas mixture was completely removed by the reaction. At the end of reaction, however, SO2 was no longer consumed and dissolved into the solution and then the SO2 concentration of outlet stream started to increase. [0052] Effects of Temperatures on the Reaction Rates [0053] The relationships between reaction temperature and the reaction time needed for the completion of reactions at given reaction conditions are shown in FIG. 1. FIG. 1 shows that the higher the reaction temperature is the shorter the reaction time needed. This fact can be explained with kinetic theory that higher temperature results in a higher reaction rate constant. It can be seen that reaction times at a temperature of 60° C. were about 75% of those at 30° C. In real-world industrial applications with fixed SO2 flow rates, higher temperatures may yield higher recovery rates-but also a higher levels of energy consumption. [0054] Effects of SO2 Concentrations on the Reaction Rates [0055] SO2 concentrations directly affected reaction times. Higher SO2 concentrations shortened the amount of time needed to complete reactions in the system. FIG. 4 shows that reaction time decreased as the SO2 flow rate increased-an obvious outcome, since the high SO2 concentrations represent that more SO2 was sparged into the system over the same period. However, the reaction time was not proportional to the flow rate at which SO2 was sparged into the system. The results showed that reaction times under the condition of 3.0 v % of SO2 concentration were only about 80% greater than those with a concentration of 9.0 v %, assumed previously to be up to 200% greater if SO2 concentrations determined reaction time. This indicates that reaction in the system was complex, and that the reaction rate was not controlled solely by means of the SO2 flow rate. [0056] The concentrations of acetic acids produced under different reaction conditions are listed in the Table 1. It shows that SO2 concentration and reaction temperature had no substantial effect on the concentrations of acetic acid produced. Although there were some deviations from the designed 1.667 M of acetic acid concentration, these differences were random and no indication of effects from these two factors could be found. This result suggests that high concentrations of SO2 can be used to recover acetic acid from the calcium acetate solution at room temperature. Since reaction at room temperature would save large amounts of the energy needed to heat for reaction, both of these conditions are highly desirable in real-world industrial applications, albeit at the cost of longer reaction times. Increasing SO2 concentrations, however, can make up this deficiency. Large amount of gas stream containing high concentration of SO2 is available in new generation of power plants [15, 16], which will make the recovery of acetic acid from biostreams with SO2 feasible. [TABLE-US-00001] TABLE 1 The concentrations of produced acetic acid (M)based on temperature and SO2 concentration Temperature (° C.)SO2 Concentration (v %) 20 30 40 50 60 3.0 1.636 +/- 1.561 +/- 1.606 +/- 1.671 +/- 1.629 +/- 0.030 0.017 0.024 0.012 0.026 4.5 1.666 +/- 1.721 +/- 1.624 +/- 1.702 +/- 1.658 +/- 0.012 0.029 0.049 0.029 0.036 6.0 1.669 +/- 1.650 +/- 1.661 +/- 1.665 +/- 1.666 +/- 0.050 0.053 0.055 0.035 0.008 7.5 1.658 +/- 1.692 +/- 1.679 +/- 1.658 +/- 1.647 +/- 0.013 0.029 0.063 0.013 0.012 9.0 1.673 +/- 1.666 +/- 1.645 +/- 1.695 +/- 1.571 +/- 0.009 0.023 0.010 0.038 0.003 [0057] Summary [0058] Sulfur dioxide can be used to recover acetic acid efficiently from calcium acetate solutions. The experimental results show that the time required for a complete reaction decreases with an increase of reaction temperature and SO2 flow rate. Although a change of reaction conditions leads to a change of reaction time, analysis of the produced acetic acid concentrations demonstrates that the complete conversion of calcium acetate to acetic acid was not affected. This suggests that the recovery process can be designed using a higher SO2 flow rate at room temperature without affecting recovery efficiency. Since energy for heating is substantially reduced, the latter feature is economically attractive for the industrial recovery of acetic acid from biological fermentation broth. Industry can either increase the flow rate of SO2 containing gas or even use pure SO2 gas. [0059] For the above-stated reasons, it is submitted that the present invention accomplishes at least all of its stated objectives. [0060] Having described the invention with reference to particular compositions and methods, theories of effectiveness, and the like, it will be apparent to those of skill in the art that it is not intended that the invention be limited by such illustrative embodiments or mechanisms, and that modifications can be made without departing from the scope or spirit of the invention, as defined by the appended claims. It is intended that all such obvious modifications and variations be included within the scope of the present invention as defined in the appended claims. The claims are meant to cover the claimed components and steps in any sequence which is effective to meet the objectives there intended, unless the context specifically indicates to the contrary.
  • 16
  • [ 1351764-67-4 ]
  • [ 62-54-4 ]
  • hemi calcium salt of (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-[(4-hydroxymethylphenylamino)carbohyl]-pyrrol-1-yl]-3,5-dihydroxy-heptanoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
31% In water Ia.3.b To an aqueous solution of the sodium salt of the acid (prepared by adding 1 equivalent IN sodium hydroxide solution) was added dropwise an aqueous solution (1M) of calcium acetate (0.55 equiv). White precipitate was obtained, which was filtered off and washed with copious amount of water, and dried in vacuo.
  • 17
  • C33H40FN2O5(1-)*Na(1+) [ No CAS ]
  • [ 62-54-4 ]
  • hemi calcium salt of (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-[(cyclohexylamino)carbonyl]-pyrrol-1-yl]-3,5-dihydroxy-heptanoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water II To an aqueous solution of the sodium salt of the acid (prepared by adding 1 equivalent IN sodium hydroxide solution) was added dropwise an aqueous solution (1M) of calcium acetate (0.55 equiv). White precipitate was obtained, which was filtered, washed with copious amount of water, and dried in vacuo.
  • 18
  • sodium salt of (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-[(3-acetylphenylamino)carbonyl]-pyrrol-1-yl]-3,5-dihydroxy-heptanoic acid [ No CAS ]
  • [ 62-54-4 ]
  • hemi calcium salt of (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-[(3-acetylphenylamino)carbonyl]-pyrrol-1-yl]-3,5-dihydroxy-heptanoic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
21.35% In water I.5.b; Ib.5.b To an aqueous solution of sodium salt of acid (is prepared by adding 1 equivalent IN sodium hydroxide solution) was added dropwise an aqueous solution (1M) of calcium acetate (0.55 equiv). White precipitate was obtained, which was filtered off, washed with copious amount of water, and dried in vacuo.
  • 19
  • (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-(3-fluorophenylamino)-carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid sodium salt [ No CAS ]
  • [ 62-54-4 ]
  • (3R,5R)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-[(3-fluorophenylamino)-carbonyl]-1H-pyrrol]-3,5-dihydroxy-1-heptanoic acid calcium salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
32% In water I.5.b Scheme I; Step 5: Preparation of Hemi Calcium Salt of Formula I To an aqueous solution of sodium salt of acid (prepared by adding 1 equivalent 1N sodium hydroxide solution) was added dropwise an aqueous solution (1M) of calcium acetate (0.55 equiv). A little white precipitate was obtained which was filtered off and washed with copious amout of water, dried in vacuo. The following compounds were prepared following above general procedure: (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(3-fluorophenylamino) carbonyl]-1H-pyrrol-3,5-dihydroxy 1-heptanoic acid calcium salt(Compound No. 3), 1H NMR(DMSO-d6, 300 MHz):δ1.21 (brs-2H), 1.37 (brs, 6H), 1.53 (brs, 2H), (brs, 1H), 2.00 (brs, 1H), 3.25 (brs, 1H), 3.38 9brs, 1H), 3.70 (brs, 2H), 3.94 (brs, 1H), 6.81 (brs, 1H), 7.06 (brs, 4H), 7.23 (brs, 6H), 7.52 (brs, 2H), 10.11 (s, 1H, d2O exchanged) MS (+ve ion mode): m/z 578 [acid+1] Yield: 32% m.pt: 224.5-229 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(4-fluorophenylamino) carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt(Compound No. 4), 1H NMR(DMSO-d6):δ1.23 (brs, 2H), 1.37 (d, J=5.7Hz, 6H), 1.56 (brs, 2H), 1.88-2.10 (m, 2H), 3.52 (brs, 1H), 3.73 (brs, 2H), 3.95 (brs, 1H), 7.06 9brs, 1H), 7.12-7.38 (brm, 4H), 7.53 9brs, 2H), 9.90 (s, 1H) d2O exchange MS (+ve ion mode): m/z 577 [Acid+1] Yield: 18% m.pt. 196.4-201.6 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(pyridin-3-yl-amino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 6), 1H NMR(DMSO-d6, 300 MHz):δ1.24 (brs, 2H), 1.37 (d, J=6.0Hz, 6H), 1.5-1.70 (m, 2H), 1.94 (dd, J=15.0 & 6.0H, 1H), 2.05 (dd, J=12Hz & 3.0Hz, 1H), 3.51 (brs, 2H), 3.74 (brs, 2H), 3.90-4.20 (m, 1H), 4.6-4.9 (brs, 1H (D20 exchange)), 7.0-7.11 (m, 5H), 7.16-7.25 (m, 5H), 7.95 (d, J=9.0Hz, 1H), 8.19 (d, J=6.0Hz, 1H), 8.6 s, 1H), 10.03 (s, 1H) MS (+ve ion mode): m/z 560.4 [Acid+1] Yield: 22% (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(pyridin-4-yl-amino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt(Compound No. 7), 1H NMR(DMSO-d6, 300 MHz):δ1.24 (brs, 2H), 1.36 (d, J=6.0Hz, 6H), 15-175 (m, 2H), 192 (dd, J=15.0 & 6.0H, 1H), 2.0-212 (m, 1H), 3.1-3.55 (m, 2H), 3.74 (brs, 2H), 4.0 (brs, 1H), 6.87-7.07 (m, 5H), 716-7.25 (m, 4H), 7.48 (d, J=60H, 2H), 8.32 (d, J=3.0Hz, 2H), 10.23 (s, 1H) MS(+ve ion): m/z 560.1 [acid+1]+Yield: 7% Melting Point ( C.): 212.9-215.2 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(4-cyanophenylamino) carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 9), 1H NMR (DMSO-d6):δ1.12-1.42 (brs, 8H), 1.55 (m, 2H), 1.84-2.10 (m, 2H), 3.52 (brs, 1H), 3.75 (brs, 2H), 3.96 (brs, 1H), 6.95-7.30 (m, 9), 7.70 (brs, 4H), 10.28 (s, 1H, d2O exchanged) MS (+ve ion mode): m/z 584 [Acid+1] Yield: 30.05% m.pt: 209-249 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-phenyl-4-[(2,4-difluorophenylamino) carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 10), 1H NMR(DMSO-d6, 300 MHz):δ1.23 (brs, 2H), 1.36 (d, J=6Hz, 6H), 1.50-1.75 (m, 2H), 1.90-2.20 (m, 2H), 3.51 (brs, 1H), 3.71 (brs, 2H), 3.95 (brs, 1H), 7.06 (brs, 5H), 7.15-7.24 (m, 4H), 7.52 (brs, 2H), 9.93 (5, 1H) MS (+ve ion mode): m/z 595 (acid+1) Yield: 34.02% Melting Point=249.5-272.8 C. (3R,5R)-7-[2-(2,4-Difluorophenyl)-5-isopropyl-3-phenyl-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 12), 1H NMR(DMSO-d6, 300 MHz):δ1.14 (brs, 2H), 1.30 (d, J=6Hz, 6H), 1.44 (brs, 2H), 1.82 (dd, J=14.1 & 7.2Hz, 1H), 1.94-1.98 (m), 3.17 (sept, J=7.2Hz, 1H), 3.45 (brs, 1H), 3.74 (brs, 1H), 3.82 (brs, 1H), 3.86 (brs, 1H), 6.89-7.07 (m, 7H), 7.12-7.28 (m, 4H), 7.46 (d, J=7.8Hz, 2H) MS (+ve ion mode): m/z 577 (acid+1)+Yield: 29% Melting point C.=203.6-217.4 C. (3R,5R)-7-[2-(3,4-Difluorophenyl)-5-isopropyl-3-phenyl-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 13), 1H NMR(DMSO-d6, 300 MHz):δ1.21-1.26 (m, 1H), 1.36 d, J=6.6Hz, 6H), 1.32-1.45 (m, 3H), 191 (dd, J=15 & 6Hz, 1H), 2.06 (dd, J=14.7 & 4Hz, 1H), 3.21-3.54 (m, 2H), 3.57-4.02 (m, 3H), 6.96-7.13 (m, 7H), 7.19-7.27 (m, 3H), 7.39-7.52 (m, 3H), 9.87 (s, 1H). MS (+ve ion mode): m/z 576 (Acid+1) Yield: 66% m.p.=169-231 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-(2,4-difluorophenyl)-4-[(phenylamino) carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 15), 1H NMR(DMSO-d6):δ1.27 (brs, 2H), 1.38 (d, J=5.86Hz, 6H), 1.57 (brs, 2H), 1.88-2.13 (m, H), 3.27 (brs, 1H), 3.55 (brs, 1H) (brs, 2H) 4.00 (brs, 1H), 6.83-7.03 (m, 3H), 7.17 (brs, 7H), 7.45 (brs, 2H), 9.63 (s, 1H, D2O exchanged) MS (+ve ion mode): m/z 596 [Acid+1] Yield 31% m.p. 172.8-221.1 C. (3R,5R)-7-[2,3-Di-(4-fluorophenyl)-5-isopropyl-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt(Compound No. 16), 1H NMR(DMSO-D6):δ1.09 (brs, 2h), 1.21 (D, 5=6.5Hz, 6H), 1.57 (brs, 2H), 1.85-2.20 (m, 2H), 3.22 (brs, 1H), 3.37 (brs, 1H) (brs, 2H) 3.76 (brs, 1H), 6.85-7.12 (m, 5H), 7.13-7.35 (m, 6H), 7.48-7.65 (m, 2H), 9.87 (s, 1H, d2O exchanges) MS (+ve ion mode): m/z 578 [Acid+1] m.p. 175.7-212.4 C. yield 20% (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-(4-methylphenyl)-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 17), 1H NMR(CDCl3):δ1.24 (brs, 2H), 1.36 (d, 6H, J=9Hz), 1.56 (brs, 2H), 1.89-2.22 (m, 5H), 3.21 (brs, 2H), 3.52 (bras, 1H), 3.74 (bras, 2H), 3.94 (brs, 1H), 6.85-7.05 (m, 5H), 7.15-7.30 (m, 6H), 7.54 (d, J=6Hz, 2H), 9.87 (s, 1H, d2O exchanged) MS (+ve ion mode): m/z 574 [Acid+1] Yield: 40% m.pt. 195-217.4 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-isopropyl-3-(4-trifluoromethylphenyl)-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 18), 1H NMR(DMSO):δ1.26 (brs, 2h), 1.38 (D, j=6Hz, 6H), 1.62 (brs, 2H), 1.95-220 (m, 2H), 3.25 (brs, 1H), 3.54 (brs, 1H) (brs, 2H), 4.05 (brs, 1H), 7.0 (t, J=7.1Hz, 1H), 7.25 (brs, 8H), 7.45 (d, J=7.8Hz, 2H), 7.54 (d, J=7.6Hz, 2H), 10.02 (s, 1H, d2O exchanged) MS (+ve ion mode): m/z 628 [Acid+1] Yield 17%, m.p 174.3-221.3 C. (3R,5R)-7-[2-(4-Fluorophenyl)-5-cyclopropyl-3-phenyl-4-[(phenylamino)carbonyl]-1H-pyrrol-3,5-dihydroxy-1-heptanoic acid calcium salt (Compound No. 19), 1H NMR(DMSO-d6, 300 MHz):δ0.63 (brs, 2H), 0.82 (brs, 2H), 1.15-1.44 (m, 2H), 1.88-2.10 (m, 3H), 3.51 (brs, 1H), 3.72 (brs, 1H), 3.90-4.11 (m, 2H), 6.99-7.09 (m, 6H), 7.14-7.32 (m, 6H), 7.60 (d, J=6Hz, 2H), 10.04 (s, 1H). MS (+ve ion mode): m/z 557 (M++1) Yield=26% m.p.=160-230 C.
  • 20
  • [ 64-19-7 ]
  • calcium carbonate [ No CAS ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
In water for 2.5h; 8.1 Preparation of Calcium Acetate. One liter (17.48 moles) of acetic acid was added to an eight-liter container, and one liter of water was added. Calcium carbonate powder (874 g, 8.74 mole, 99+%) was added in 100-g portions over 2.5 hours with agitation until the solution was neutral to pH paper. Water was added as needed to maintain fluidity in the mixture during the neutralization
In acetic acid byproducts: H2O, CO2; kinetic of CaCO3 dissolution in acetic acid at temp. 283-343 K was studied; elem. anal.;
In water gray lime production: CaCO3 from production of acetone; concg. to dryness;;
In acetic acid addn. of acetic acid (even diluted) to CaCO3 (chalk or oyster shells) at ambient temp. or faster and more complete at elevated temp.;;
In water gray lime production: treatment of raw acetic acid; concg. to dryness;;
In acetic acid addn. of pure CaCO3 to pure glacial CH3CO2H, until saturation; filtration; vaporization on sand bath, until formation of crust on surface; vaporization to dryness on water bath; solving residue in hot H2O, vaporization until formation of thick crust;; drying of crust on water bath and over night in electric furnace at 120°C; free of organic calcium salts and basic salts, contains 5-6% water and 2.0-2.4% free acetic acid; large degree of dehydration by heating;;
In water gray lime production: CaCO3 from production of acetone dissolved in hot water or Ca acetate soln.;;
In water gray lime production: CaCO3 from production of acetone; concg. to dryness;;
In water gray lime production: treatment of raw acetic acid; concg. to dryness;;
In acetic acid addn. of acetic acid (even diluted) to CaCO3 (chalk or oyster shells) at ambient temp. or faster and more complete at elevated temp.;;
In acetic acid addn. of pure CaCO3 to pure glacial CH3CO2H, until saturation; filtration; vaporization on sand bath, until formation of crust on surface; vaporization to dryness on water bath; solving residue in hot H2O, vaporization until formation of thick crust;; drying of crust on water bath and over night in electric furnace at 120°C; free of organic calcium salts and basic salts, contains 5-6% water and 2.0-2.4% free acetic acid; large degree of dehydration by heating;;
In water gray lime production: CaCO3 from production of acetone dissolved in hot water or Ca acetate soln.;;

  • 21
  • [ 6553-96-4 ]
  • phosphoric acid mono(3-dodecylmercapto-2-decyloxy)-1-propyl ester [ No CAS ]
  • [ 47066-33-1 ]
  • [ 62-54-4 ]
  • (6-Mercaptopurine-9-β-D-ribofuranoside)-5'-phosphoric acid (3-dodecylmercapto-2-decyloxy)propyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water 2 (6-Mercaptopurine-9-β-D-ribofuranoside)-5'-phosphoric acid (3-dodecylmercapto-2-decyloxy)propyl ester EXAMPLE 2 (6-Mercaptopurine-9-β-D-ribofuranoside)-5'-phosphoric acid (3-dodecylmercapto-2-decyloxy)propyl ester 6.2 g (12.5 mmoles) of phosphoric acid (3-dodecylmercapto-2-decyloxy)propyl ester was treated with 5.7 g (18.75 mmoles) of 2,4,6-triisopropylbenzenesulfonic acid chloride as described in example 1 and subsequently with 3.55 g (11.25 mmoles) of 6-mercaptopurine-9-β-D-ribofuranoside and after 24 hours, this was hydrolyzed with water. Then, 2.85 g of calcium acetate in 15 ml of water was slowly dropped therein, precipitating the crude calcium salt of the conjugate. After prolonged stirring the precipitate with acetone (1/10), 6 g of an amorphous crude product was obtained, having 72 area % according to HPLC. The calcium salt was suspended in 350 ml of methanol, treated with 150 g of Amberlite IR 120 in the Na+ form and stirred for 2 days. Thereafter, the ion exchanger was removed, the filtrate was evaporated, and the residue was purified by column chromatography on LiChroprep RP-18 with a linear gradient of methanol/water 5/1 to 9/1. The fractions containing product were evaporated in a vacuum, and the residue was stirred with acetone and dried. Yield: 3.52 g (41% of theoretical amount). DC; Rf =0.45 (isopropanol/butyl acetate/conc. ammonia/water 50/30/5/15).
  • 22
  • [ 14297-60-0 ]
  • [ 62-54-4 ]
  • dimethyl 2,5-di-hydroxy-cyclohexadiene-1,4-dicarboxylate [ No CAS ]
YieldReaction ConditionsOperation in experiment
91.6% 2 EXAMPLE 2 EXAMPLE 2 The procedure is as described in Example 1, but instead of magnesium acetate tetrahydrate, 0.337 part of calcium acetate (94% pure) is added. 172.4 parts of dimethyl 2,5-di-phenylamino-terephthalate (corresponding to a yield of 91.6%, based on the dimethyl 2,5-di-hydroxy-cyclohexadiene-1,4-dicarboxylate employed) with a melting point of about 159° to 162° C. are obtained.
  • 23
  • (6R,S)-tetrahydrofolic acid [ No CAS ]
  • [ 96-27-5 ]
  • [ 62-54-4 ]
  • calcium salt of (6R,S)-tetrahydrofolic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water 5 Example 5 Example 5 ›Am[593] 4.0 g (6R,S)-tetrahydrofolic acid were slurried under nitrogen in 40 ml water containing 0.4 g thioglycerol, the pH was adjusted to 8.5 with 30% aqueous sodium hydroxide solution, and the slurry was treated with 2.0 g calcium acetate at 50° C. The beige product which slowly crystallized out from the resulting solution was filtered off under suction and the residue was washed with water. After drying, 3.64 g of the crystalline calcium salt of (6R,S)-tetrahydrofolic acid was obtained, which had a (6S)- fraction of 50.5% and a content amounting to 94.6% (as the salt, with respect to the dry substance). The calcium content amounted to 1.12 equivalents.
  • 24
  • [ 64-19-7 ]
  • calcium oxide [ No CAS ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
In water 7 The method of Example 1 was repeated using formic acid, acetic acid and water. The analysis of the products calcium formate and calcium acetate was: Calcium formate Calcium acetate % formate 65. 4 % acetate-71.8 % calcium 34.9 23.2 % water 1.3 2.3
In water gray lime production: treatment of raw acetic acid;;
In acetic acid addn. of acetic acid (even diluted) to CaO at ambient temp. or faster and more complete at elevated temp.;;
In acetic acid addn. of acetic acid to CaO; various temp.;;
In water gray lime production: treatment of raw acetic acid; concg. to dryness;;
In water gray lime production: treatment of raw acetic acid; concg. to dryness;;
In water gray lime production: treatment of raw acetic acid;;
In acetic acid addn. of acetic acid to CaO; various temp.;;
In acetic acid addn. of acetic acid (even diluted) to CaO at ambient temp. or faster and more complete at elevated temp.;;

  • 25
  • (S)-4-[cis-2,6-dimethyl-4-(4-trifluoromethoxy-phenyl)-piperazine-1-sulfonyl]-indan-2-carboxylic acid [ No CAS ]
  • [ 62-54-4 ]
  • C2H3O2(1-)*C23H24F3N2O5S(1-)*Ca(2+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
In methanol 3 Calcium; Compound 1 and base (Ca(OAc)2) were combined in 1:1 molar ratio in methanol solvent. No precipitation occurred, so the solution was allowed to evaporate. White solids and broken glass formed upon drying. Ether solvent was added; most of the solid dissolved, so the solution was placed in a freezer for 1 day, resulting in a clear solution with few solids. This solution was left to evaporate under ambient conditions, yielding solids with areas of birefringence.
  • 26
  • potassium phosphate [ No CAS ]
  • [ 62-54-4 ]
  • calcium hydroxyapatite [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water at 20℃; for 0.0333333h; 1 Calcium acetate hydrate (99% Acros Organics, Belgium, CAS No. 114460-21-8) and potassium orthophosphate hydrate (Acros Organics, Belgium, CASNo. 27176-10-9) were used as reactants for the synthesis of hydroxyapatite. First, a 1.0 molal calcium acetate hydrate solution was made using distilled, deionized water. Then, a 0.6 molal solution of potassium orthophosphate hydrate was made using distilled, deionized water. Equal volumes of each were then measured out for the reaction to create a calcium to phosphate ratio of 1.67 (final concentrations of ions if they were to remain in solution would be 0.5m/0.3m). A 100 mL reaction required 5OmL of the calcium solution to be measured and poured into a beaker and 5OmL of the phosphate solution to be added. Agitation via vortexing was then performed until and through the gelation stage. Once the gel returned to solution, the slurry was then allowed to age for 2 minutes. The concentrate was then dried in an oven at 7O0C for 24 hours and desiccated until use or immediately atomized onto a Transmission Electron Microscopy (TEM) grid for characterization.
  • 27
  • [ 64-19-7 ]
  • calcium hydroxide [ No CAS ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
In acetic acid sample dissoln. in AcOH glaciale, heating on steam bath;
In water gray lime production: treatment of raw acetic acid described; neutralisation with milk of lime;; purification via destillation;;
In water gray lime production: apparatus described;;
In water gray lime production: treatment of raw acetic acid described; neutralisation with milk of lime;;
In water gray lime production: treatment of raw acetic acid;;
In not given gray lime production in presence of H3PO4 or catalysts;;
In not given gray lime production in presence of H3PO4 or catalysts;;
In water gray lime production: apparatus described;;
In water gray lime production: treatment of raw acetic acid described; neutralisation with milk of lime;; purification via destillation;;
In water gray lime production: treatment of raw acetic acid described; neutralisation with milk of lime;;
In water gray lime production: treatment of raw acetic acid;;

  • 28
  • [ 62-54-4 ]
  • [ 7440-70-2 ]
  • calcium hydroxide [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water byproducts: H2; Electrolysis; at 35-37 °C;
In water byproducts: H2; Electrolysis; at 35-37 °C;
  • 29
  • [ 1633-05-2 ]
  • [ 142-71-2 ]
  • [ 62-54-4 ]
  • [ 22306-37-2 ]
  • BiCaSrCu2O(x) [ No CAS ]
  • 30
  • disodium hydrogenphosphate [ No CAS ]
  • [ 10049-21-5 ]
  • [ 62-54-4 ]
  • octacalcium phosphate pentahydrate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water mixed dropwis at pH=5, stirred at 60°C for 3 h; XRD, SEM;
In water pptd. by dropping 0.04 M soln. of Ca salt into soln. of na salts mixt.; stirred at 60°C and pH 5; ppt. washed (disd. H2O), dried at 37°C; detd. by SEM, TEM, SAED;
  • 31
  • [ 62-54-4 ]
  • [ 543-94-2 ]
  • [ 6046-93-1 ]
  • [ 22306-37-2 ]
  • (bismuth)2(strontium)2(calcium) cuprate [ No CAS ]
  • 32
  • [ 62-54-4 ]
  • manganese(II) acetate [ No CAS ]
  • [ 917-70-4 ]
  • lanthanum calcium manganes oxide [ No CAS ]
YieldReaction ConditionsOperation in experiment
With air In acetic acid acetates of Ln, Ca and Mn dissolved in a soln. of AcOH, evapd. at 110°C, pyrolysed at 600°C for 6 h with a heating rate of 75°/h, annealed at 1200°C for 48 h, pressed, sintered at 1350°C for 48 h;
With Al2O3 In water; acetic acid La(CH3CO2)3, Ca(CH3CO2)2, Mn(CH3CO2)2 dissolved in CH3CO2H and H2O, stirred at 80°C for 1 h, Al2O3 immersed at room temp. for 1 h, dried at 150°C for 6 h, heated in air at 675°C for 1 h; aq. soln. of NaOH immersed at room temp. for 24 h, diluted with H2O;
In not given synthesized by chem. soln. deposition method, polycrystalline material pressed by spark plasma sintering technique, heated in air at 800°C for about 24 h;
  • 33
  • [ 62-54-4 ]
  • calcium carbonate [ No CAS ]
YieldReaction ConditionsOperation in experiment
thermal decompn. under N2 between 315 and 490°C;
With urea; sodium bis-2-ethylhexyl-sulfosiccinate In water High Pressure; Ca(OAc)2 and urea solns. mixed, treated with 2.5 mM of sodium bis-ethylhexyl-sulfosuccinate, stirred for 15-20 min, heated in an autoclave at 150°C for 12 h; cooled to room temp., washed (H2O, alcohol) several times, dried at roomtemp. for 24 h (vac.), XRD;
at 549.84℃; Inert atmosphere;
  • 34
  • calcium(II) nitrate tetrahydrate [ No CAS ]
  • [ 108-24-7 ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
71% In acetic anhydride byproducts: NO2, Ca(NO3)2; heating a clear soln. of 6 g Ca(NO3)2*4H2O and 30 ml acetic anhydride; pptn.;; storage for some time in 96% ethanol, to remove Ca(NO3)2; sucking off; dehydration by 2 h heating in vac. at 130°C;;
71% In acetic anhydride byproducts: NO2, Ca(NO3)2; heating a clear soln. of 6 g Ca(NO3)2*4H2O and 30 ml acetic anhydride; pptn.;; storage for some time in 96% ethanol, to remove Ca(NO3)2; sucking off; dehydration by 2 h heating in vac. at 130°C;;
  • 35
  • [ 62-54-4 ]
  • mercury [ No CAS ]
  • Hg(b),Ca(0.09) (W%) [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water byproducts: H2, Ca(OH)2; Electrolysis; electrolysis of aq. satd. Ca(CH3CO2)2 soln. with Hg cathode for 40 mins at 10 V and 1.25 A with stirring, cooling with H2O, addn. of Ca(CH3CO2)2 now and then, H2 development, discoloration, turbidity of soln., rise in voltage, interruption of current;; washing at once, drying; 0.091 or 0.092 wt.-% Ca;;
  • 36
  • [ 142-71-2 ]
  • [ 62-54-4 ]
  • [ 543-94-2 ]
  • [ 301-04-2 ]
  • [ 22306-37-2 ]
  • bismuth methacrylate [ No CAS ]
  • strontium methacrylate [ No CAS ]
  • copper(II) 2-methylacrylate [ No CAS ]
  • calcium 2-methylacrylate [ No CAS ]
  • lead dimethacrylate [ No CAS ]
  • 37
  • [ 62-54-4 ]
  • tin(II) acetate [ No CAS ]
  • calcium bis[triacetatostannate(II)] [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water; acetic acid excess of Ca(CH3CO2)2, boiling in N2 atm, evapn. and cooling; washing with acetone and ether, drying over KOH in vac.;
In water; acetic acid equimolar ratio of educts, boiling in N2 atm, evapn. and cooling; washing with acetone and ether, drying over KOH in vac.;
In water; acetic acid excess of Ca(CH3CO2)2, boiling in N2 atm, evapn. and cooling; washing with acetone and ether, drying over KOH in vac.;
With AcOH In water; acetic acid N2-atmosphere; addn. of 1 equiv. of aq. Ca(OAc)2 to Sn(OAc)2 (in 60 % aq. AcOH), refluxing; concn., filtration, crystn. on cooling, filtration, washing (Me2CO, Et2O), drying (vac., over KOH); elem. anal.;

  • 38
  • [ 147-71-7 ]
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • calcium l-tartrate*4H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
98.95% In acetic acid addn. of 15 ml 95 % ethanol to mixture of 50 ml 1 % l-tartaric acid soln. and 10 ml Ca(CH3CO2)2 soln. (preparation for 1 l: 32 g CaCO3, 120 ml pure acetic acid, rest H2O); add. of further 15 ml 95 % ethanol after 24 hs; complete pptn. after 48 hs;; washing 3 times by decantation, pressing on filter paper, drying at ambient temp.;;
In acetic acid addn. of 1 l acetic Ca(CH3CO2)2 soln. (32 g CaCO3, 120 ml pure acetic acid, rest H2O) to 2 l 1 % d-tartaric acid soln.; complete pptn. after 24 hs;; washing 3 times by decantation, pressing on filter paper, drying at ambient temp.;;
In acetic acid
  • 39
  • [ 87-69-4 ]
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • calcium d-tartrate*4H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
98.95% In acetic acid addn. of 15 ml 95 % ethanol to mixture of 50 ml 1 % d-tartaric acid soln. and 10 ml Ca(CH3CO2)2 soln. (preparation for 1 l: 32 g CaCO3, 120 ml pure acetic acid, rest H2O); add. of further 15 ml 95 % ethanol after 24 hs; complete pptn. after 48 hs;; washing 3 times by decantation, pressing on filter paper, drying at ambient temp.;;
In acetic acid addn. of 1 l acetic Ca(CH3CO2)2 soln. (32 g CaCO3, 120 ml pure acetic acid, rest H2O) to 2 l 1 % d-tartaric acid soln.; complete pptn. after 24 hs;; washing 3 times by decantation, pressing on filter paper, drying at ambient temp.;;
In acetic acid
  • 40
  • [ 62-54-4 ]
  • [ 64-19-7 ]
  • calcium acetate acetic acid solvate [ No CAS ]
YieldReaction ConditionsOperation in experiment
storage of dry, H2O free calcium acetate for 1 month (in summer) over pure acetic acid;;
In water at 80℃; D) Calcium acetate acetic acid crystals, Ca(OAc)2(HOAc), from calciumacetate monohydrate In a similar procedure as used for CMA, above, several milligramsof calcium acetate monohydrate were suspended in glacial acetic acid ina 5 mL scintillation vial. Water and acetic acid were completely boiledoff. The process was repeated twice to assure that all water wascompletely removed from the sample. The white residue was takenup again in glacial acetic acid (ca 1 mL) and heated to ca 80 °C.Additional glacial acetic acid was added until all solid was completelydissolved when hot. Once all solid was dissolved, the vial was capped(to keep out atmospheric moisture), the hot plate switched off and thesolution was allowed to slowly cool to room temperature. Clusters ofcrystals were obtained after several hours. Individual platelets wereisolated from the heavily intergrown clusters for SC-XRD.
  • 41
  • [ 62-54-4 ]
  • [ 543-90-8 ]
  • calcium cadmium tetraacetate hexahydrate [ No CAS ]
YieldReaction ConditionsOperation in experiment
With water; copper diacetate In water Cd(OAc)2, Ca(OAc)2, and Cu(OAc)2 reacted in a satd. soln. in mole ratios 1:1:0.001; soln. was evapd. at room temp., crystals collected;
In not given
  • 42
  • [ 142-71-2 ]
  • [ 62-54-4 ]
  • [ 543-94-2 ]
  • [ 301-04-2 ]
  • [ 22306-37-2 ]
  • (bismuth)1.7(lead)0.4(strontium)2(calcium)2cuprate [ No CAS ]
  • 43
  • [ 113131-88-7 ]
  • [ 62-54-4 ]
  • Ca(II) salt of 4,4'-sebacoyl-bis(1-phenyl-3-methyl-pyrazolone-5) [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% In ethanol; water addn. of warm metal salt soln. to ethanolic ligand soln. (mole ratio 1:1); stirring; suction filtering of product; washing with H2O; leaching unreacted ligand with chloroform; drying (CaCl2); elem.anal.;
  • 44
  • [ 78-40-0 ]
  • [ 62-54-4 ]
  • hydroxyapatite [ No CAS ]
YieldReaction ConditionsOperation in experiment
In not given PO(OC2H5)3 dropwise addn. to Ca acetate, stirring (25-30°C, 12 h,40-45°C, 12 h), gelation on heating (75°C, 10 h), drying, heat treatment (1000°C); influence of alcohol addition studied; stirring (aq. HCl), washing (water); X-ray diffraction;
With ethanol In not given PO(OC2H5)3 dropwise addn. to Ca acetate, ethanol addn., stirring (25-30°C, 12 h, 40-45°C, 12 h), gelation on heating (75°C,10 h), drying, heat treatment (1000°C); influence of alcohol add ition studied; stirring (aq. HCl), washing (water); X-ray diffraction;
With methanol In not given PO(OC2H5)3 dropwise addn. to Ca acetate, methanol addn., stirring (25-30°C, 12 h, 40-45°C, 12 h), gelation on heating (75°C, 10 h), drying, heat treatment (1000°C); influence of alcohol addition studied; stirring (aq. HCl), washing (water); X-ray diffraction;
With propan-1-ol In not given PO(OC2H5)3 dropwise addn. to Ca acetate, propanol addn., stirring (25-30°C, 12 h, 40-45°C, 12 h), gelation on heating (75°C, 10 h), drying, heat treatment (1000°C); influence of alcohol addition studied; stirring (aq. HCl), washing (water); X-ray diffraction;

  • 45
  • [ 62-54-4 ]
  • manganese(II) acetate [ No CAS ]
  • [ 917-70-4 ]
  • lanthanum calcium manganite [ No CAS ]
YieldReaction ConditionsOperation in experiment
With acetic acid In 2-methoxy-ethanol 0.18 M soln. used for film deposition; spin coating speed is 4000 rpm; time 60 s; films placed on preheated hot plate and dried at 300°C for 30 min; annealed at 900°C for 2 h under flowing O2;
With O2 In 2-methoxy-ethanol; water water addn. to stoich. amts. of components soln. in 2-methoxyethanol, reflucing at 80°C for 24 h, ageing at room temp. for several d, distn., gel drying, spin coating on MgO, pyrolyzis on 400°C plate after each coating, final annealing at; 700-1000°C for 12 h in tube furnace under O2 flow; TG-DTA;
With ethylene glycol In water; acetic acid stoich. mixt. of acetates in H2O/acetic acid contg. ethylene glycol heated until formation of sol, template (anodized alumina) dipped into sol for 0.5 h, template dried at 150°C overnight, pyrolysed at 350°C; nanowires can be removed from template by dilute aq. NaOH;
With aq. oxalic acid; air In acetic acid stoich.; acetates dissolved in glacial CH3COOH, added aq. (COOH)2, the slurry filtered, dried at 80°C for 8 h, calcined at 900°C in air for 12 h, cooled, reground, pressed into pellets, sintered at 1100-1350°C for 24 h, cooled;

  • 46
  • [ 67-66-3 ]
  • (HO)2C6H2(CHNOCH2CH2ONCHC6H3(OCH3)OH)2 [ No CAS ]
  • [ 62-54-4 ]
  • [ 5970-45-6 ]
  • O2C6H2(CHNOC2H4ONCHC6H3(OCH3)O)2(4-)*2Zn(2+)*Ca(2+)*2O2CCH3(1-)*0.75CHCl3=C32H32CaN4O14Zn2*0.75CHCl3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
77% In methanol; chloroform; water a soln. of Zn salt in MeOH and a soln. of Ca salt in H2O/MeOH added to asoln. of ligand in CHCl3; evapd., crystd. by vapor diffusion of Et2O into a CHCl3/MeOH soln.; elem. anal.;
  • 47
  • [ 62-54-4 ]
  • [ 125-71-3 ]
  • dextromethorphan calcium acetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water 7 An aqueous mixture is prepared by stirring at room temperature for one hour a mixture of dextromethorphan free base (20 parts by weight); 296.3 parts by weight water and a stoichiometric excess of calcium acetate (11.7 parts by weight). The above-noted acid salt is isolated for later use by filtering the so-formed solids and oven drying the solids to produce a solid granular product. Alternatively, the solid salt also can be used directly to produce taste masked granules, for example by mixing the acid salt slurry with 43 parts by weight of a 15% by weight aqueous solution of polyethylene glycol (M.W. 3350) and then 13.7 parts macrocrystalline cellulose. The homogeneous mixture is then concentrated under vacuum (Rotovap) at 65°C to produce a solid granular product.
  • 48
  • [ 62-54-4 ]
  • [ 134523-01-6 ]
  • [ 134523-03-8 ]
YieldReaction ConditionsOperation in experiment
In methanol; water at 13 - 63℃; 1 The quantity of atorvastatin obtained by purification was determined by calibrated HPLC analysis of the purified atorvastatin sodium salt solution. Based on this analysis, a quantity of calcium acetate (8.38 g, 0.5 eq.) was dissolved in water (1.9 L) and heated to 60° C. The atorvastatin sodium salt solution was heated to 63° C. and the solutions were combined by slow addition of the calcium acetate solution to the atorvastatin sodium salt solution. Upon completing the addition, the mixture was cooled. Crystallization of Form V began to occur at a temperature of 43° C. and cooling was continued until the flask temperature reached 13° C.The crystals were isolated by slow vacuum filtration and then dried over anhydrous silica for 5 days to yield atorvastatin calcium salt Form V.
  • 49
  • [ 62-54-4 ]
  • [ 541-15-1 ]
  • L-carnitine calcium acetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
> 90% In water; for 2h; EXAMPLE 5; Preparation of <strong>[541-15-1]L-carnitine</strong> calcium acetate. A mixture of calcium acetate (0.5 g, 0.003 mol) and <strong>[541-15-1]L-carnitine</strong> (0.5 g, 0.003 mol) was dissolved in water (15 mL) and stirred for 2 hours. The clear and colorless solution was concentrated at reduced pressure at bath temperatures that were less than about 70 C. to a white solid. The solid, <strong>[541-15-1]L-carnitine</strong> calcium acetate, was obtained in greater than 90% yield and had a melting point of 166-167 C., with decomposition and evolution of trimethylamine. (The melting point of <strong>[541-15-1]L-carnitine</strong> was 186-190 C.) The solid was not hygroscopic. The solid had no objectionable taste. The 1H-Nuclear Magnetic Resonance (1H-NMR) spectrum (FIG. 1) is consistent with the structure of the salt and shows the presence of <strong>[541-15-1]L-carnitine</strong> and acetate in a molar ratio of approximately 1:2. (Calcium is not detected by 1H-NMR.)
  • 50
  • Elinogrel [ No CAS ]
  • [ 62-54-4 ]
  • calcium [4-(6-chloro-7-methylamino-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-phenyl]-5-chloro-thiophen-2-yl-sulfonylurea [ No CAS ]
YieldReaction ConditionsOperation in experiment
100% In isopropyl alcohol for 2h; 9 Example 9: Salt screen of f4-(6-fluoro-7-methylamino-2,4-dioxo-l,4-dihydro-2H- quinazolin-3-yI)-phenyI1-5-chloro-thiophen-2-yI-suIfonyIureaPrimary Screen[0303] To 20 nig of [4-(6-fluoro-7-methylamino-2,4-dioxo-l,4-dihydro-2H-quinazolin-3- yl)-phenyl]-5-chloro-thiophen-2-yl-sulfonylurea in 3 mL of the various solvents, was added 1.1 eq. of the base in 1 mL solvent. The mixture was shaken for 2 hours and the solutions were left to evaporate down to half their volume to try to precipitate out the salt. The results are presented in Table 4 below, which shows the bases used for the screen. The solutions in THF evaporated down to solids very quickly and these were analysed by XRPD. Most samples from THF were amorphous oily solids which were left to maturate at 50°C/ambient temperature. Any solutions that did not form a solid by evaporation had IPA added as an anti-solvent to induce solid to precipitate. Samples with IPA that did not precipitate were left to evaporate. As shown in Table 5 below, the solutions yielded some solids and some oils. Oils/emulsions and opaque liquids were left to maturate at 50°C/ambient in an 8 hour cycle for several weeks. Microscopy and XRPD results showed some samples were crystalline but lack of a solid meant clear diffractograms could not be obtained. Solid samples (crystalline and amorphous) were then filtered, dried and then analyzed to judge their purity, crystallinity and stability. Solids were analysed by 1H NMR to confirm salt formation and analyzed by Ion Chromatography and TGA to obtain the stoichiometry of the salt.
In tetrahydrofuran for 2h; 9 Example 9: Salt screen of f4-(6-fluoro-7-methylamino-2,4-dioxo-l,4-dihydro-2H- quinazolin-3-yI)-phenyI1-5-chloro-thiophen-2-yI-suIfonyIureaPrimary Screen[0303] To 20 nig of [4-(6-fluoro-7-methylamino-2,4-dioxo-l,4-dihydro-2H-quinazolin-3- yl)-phenyl]-5-chloro-thiophen-2-yl-sulfonylurea in 3 mL of the various solvents, was added 1.1 eq. of the base in 1 mL solvent. The mixture was shaken for 2 hours and the solutions were left to evaporate down to half their volume to try to precipitate out the salt. The results are presented in Table 4 below, which shows the bases used for the screen. The solutions in THF evaporated down to solids very quickly and these were analysed by XRPD. Most samples from THF were amorphous oily solids which were left to maturate at 50°C/ambient temperature. Any solutions that did not form a solid by evaporation had IPA added as an anti-solvent to induce solid to precipitate. Samples with IPA that did not precipitate were left to evaporate. As shown in Table 5 below, the solutions yielded some solids and some oils. Oils/emulsions and opaque liquids were left to maturate at 50°C/ambient in an 8 hour cycle for several weeks. Microscopy and XRPD results showed some samples were crystalline but lack of a solid meant clear diffractograms could not be obtained. Solid samples (crystalline and amorphous) were then filtered, dried and then analyzed to judge their purity, crystallinity and stability. Solids were analysed by 1H NMR to confirm salt formation and analyzed by Ion Chromatography and TGA to obtain the stoichiometry of the salt.
  • 51
  • [ 10049-21-5 ]
  • [ 62-54-4 ]
  • brushite [ No CAS ]
YieldReaction ConditionsOperation in experiment
With chitosan In water chitosan-coated glass substrate transferred into soln. of polyaspartic acid and calcium acetate, then NaH2PO4 soln. added and mixt. was kept at 18°C for (few min - several h); substrate washed with water and dried at room temp.; XRD;
  • 52
  • [ 74974-60-0 ]
  • [ 62-54-4 ]
  • Ga((O)2C6H3CHNNHC(O)C6H5)3Ca(1-) [ No CAS ]
  • 53
  • [ 1187856-50-3 ]
  • [ 62-54-4 ]
  • calcium 2-(((1r,4r)-4-(((3-fluorophenyl)(phenyl)carbamoyloxy)methyl)cyclohexyl)methoxy)acetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water; isopropyl alcohol at 20℃; 1.111 Example 1.111: Preparation of Calcium 2-(((lr,4r)-4-(((3- Fluorophenyl)(phenyl)carbamoyloxy)methyl)cyclohexyl)methoxy)acetate Solvate.; Ca(OAc)2 (aqueous solution, 2.13M) was added to a solution of 2-(((lr,4r)-4-(((3- fluorophenyl)(phenyl)carbamoyloxy)methyl)cyclohexyl)methoxy)acetic acid in IPA (64.456 mg/mL) at room temperature to achieve a 1:2 ratio of calcium to 2-(((lr,4r)-4-(((3- fluorophenyl)(phenyl)carbamoyloxy)methyl)cyclohexyl)methoxy)acetic acid. A white precipitate formed immediately. The solid was isolated by filtration. The TGA thermogram of the title compound (Figure 20) shows a weight loss of about 8.2%, indicating that the compound is a solvate. The PXRD pattern for the solvate is shown in Figure 21.
  • 54
  • [ 355805-96-8 ]
  • [ 62-54-4 ]
  • crestor [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: rosuvastatin methylamine salt With sodium hydroxide In water at 25 - 30℃; for 0.333333h; Stage #2: calcium acetate In water at 20 - 22℃; for 0.333333h; Example 16: Preparation of amorphous rosuvastatin calcium Rosuvastatin methyl ammonium salt (10 gm) was added in water (50 ml) and sodium hydroxide solution (8%, 9.0 ml) was added to it at 25-30°C and stirred for 20 minutes. The solution was filtered through celite bed and the bed was washed with water (20 ml). From the resulting clear filtrate, water was removed (about 40 ml) by vacuum distillation at about 60°C. To the resulting solution, water (40 ml) and a solution of calcium acetate (2 gm) in water (10 ml) was added at 20-22°C under vigorous stirring. Solid rosuvastatin calcium precipitates out from reaction mass. To the reaction mass, tetrahydrofuran (50 ml) was added and stirred for 10 minutes. Sodium chloride (2.0 gm) was added to the reaction mass and stirred for further 10 minutes. The layers were separated and the organic layer was dried over powdered molecular sieves (10 gm). The molecular sieves were removed by filtration and the resultant solution was distilled azeotropically to remove water. After complete removal of water, tetrahydrofuran (50 ml) was added and the solution was filtered through celite bed. The clear filtrate was then concentrated under vacuum to get amorphous form of rosuvastatin calcium which was dried at 45°C under vacuum. Yield: 7.6 gm
  • 55
  • [ 62-54-4 ]
  • [ 503610-43-3 ]
  • crestor [ No CAS ]
YieldReaction ConditionsOperation in experiment
75% Stage #1: Rosuvastatin lactone With sodium hydroxide In methanol; water for 3h; Stage #2: calcium acetate In water at 20 - 22℃; for 2h; 15 Example 15: Preparation of amorphous rosuvastatin calcium Rosuvastatin lactone as obtained in step a) of Example 13 was dissolved in methanol (100 ml) and water (100 ml). To this solution, 8% sodium hydroxide solution was added till the pH of the reaction mass was about 8.5 to 8. 7 and stirred for further 3 hours. After ensuring the absence of rosuvastatin lactone by TLC, the solvent was removed under vacuum and the aqueous layer was washed with methyl tert-butyl ether (80 ml). The traces of methyl tert-butyl ether were removed under vacuum and to the aqueous layer, a solution of calcium acetate (4.0 gm) in water (25 ml) was added at 20-22°C with vigorous stirring. After complete addition, the mixture was stirred for further 2 hours at 20-22°C and filtered, washed the cake with water (20 ml) thrice and then dried at 45°C under vacuum to get the amorphous rosuvastatin calcium. Yield: 13. 8 gm (75%)
  • 56
  • tetrabutoxytitanium [ No CAS ]
  • [ 127-09-3 ]
  • [ 62-54-4 ]
  • [ 22306-37-2 ]
  • Ca0.18Na0.32Bi0.50TiO3 [ No CAS ]
  • 57
  • titanium-oxy-acetylacetonate [ No CAS ]
  • C6H3(OH)2CHNNHS(O)2C6H4CH3 [ No CAS ]
  • [ 62-54-4 ]
  • Ti(4+)*Ca(2+)*3C6H3(O)2CHNNHS(O)2C6H4CH3(2-)=[TiCa(C6H3(O)2CHNNHS(O)2C6H4CH3)3] [ No CAS ]
YieldReaction ConditionsOperation in experiment
82% With K2CO3 In methanol; water to flask charged with soln. (CH3OH) of tosylhydrazone and Ca compd. added aq. soln. of Ti and K compds., stirred for 72 h; excess of K2CO3 filtered off, solvent evapd. under reduced pressure;
  • 58
  • [ 62-54-4 ]
  • [ 287714-41-4 ]
  • crestor [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water; at 20℃; for 2.5h; The detailed preparation process is as follows: 80mL acetonitrile was added to a 200mL reaction flask and stirred. Subsequently, 12.5g (3R,5S,6E)-7-[4-(4-flurophenyl)-6-(1-methyl ethyl)-2-[methyl (methyl sulfonyl) amino]-5-pyrimidyl]-3,5-dihydroxy-6-heptenoic-3-methyl butyrate was added to the flask and heated to 35C, and then 25mL purified water was added. 25mL 1N sodium hydroxide solution was slowly added at constant speed at 40C, wherein the addition took 15 minutes. The mixture was kept at 40C and reacted for 2.5 hours. The obtained mixture was vacuum distilled at 40C to remove acetonitrile. 25mL purified water was added to the residue, the pH value was adjusted to 9 with 3g 0.5N glacial acetic acid solution, and the mixture was then cooled to 0C in an ice-salt bath. The water phase was washed for three times with ethyl ether (30mL each time), the water phase was stirred for 15 minutes during each washing, and then it was allowed to stand for layering. Then the temperature was increased to 40C, vacuum distillation was carried out to remove remaining ethyl ether, the water phase was filtered to a salt reaction flask and washed with 20mL purified water. The washing solution and filtrate were combined and cooled to 20C. Then 13.5mL 1N filtered calcium acetate was slowly added at constant speed. The addition process took about 30 minutes, and the mixture was stirred for 2 hours at 20C. It was then filtered, the obtained solid was treated with 40mL 20C purified water. It was then vacuum dried. As a result, 7.3g <strong>[287714-41-4]Rosuvastatin</strong> calcium was obtained.Furthermore, after the removal of <strong>[287714-41-4]Rosuvastatin</strong> calcium by precipitation, a certain amount of <strong>[287714-41-4]Rosuvastatin</strong> calcium still remained in the mother liquid. Therefore, the present invention also preferably provides a method for the recovery of <strong>[287714-41-4]Rosuvastatin</strong> calcium in the mother liquid. The mother liquid was transferred to a 1000mL reaction flask, 200mL ethyl ether was added, at the same time the pH value was adjusted with 0.5N hydrochloric acid until it reached 3. Then the mixture was stirred for 15 minutes and allowed to stand for layering. The water phase was washed twice with ethyl ether (100mL each time), during each washing the water phase was stirred for 15 minutes, and then it was allowed to stand for layering, the organic phase was combined and washed twice with purified water (150mLx2), during each washing the organic phase was stirred for 15 minutes. It was then allowed to stand for layering. The water phase was removed, while 4g anhydrous sodium sulfate was added to the organic phase and stirred for 30 minutes, the obtained mixture was filtered to remove anhydrous sodium sulfate, and the filtrate was then condensed. The obtained solution was vacuum distilled to remove ethyl ether until 300mL ethyl ether was distilled at 40C. Subsequently, 40mL purified water was added to the residue, the obtained was cooled to 30C with icy water, 8.4mL 1N NaOH solution was added slowly at 40C until the pH reached 11. The mixture was then stirred for 60 minutes, the pH value was adjusted to 9 with 2g 0.5N glacial acetic acid, and the obtained mixture was allowed to stand for layering. The water phase was washed twice with ethyl ether (10mL each time), during each washing the water phase was stirred for 15 minutes, then it was allowed to stand for layering. The water phase was vacuum distilled at 40C to remove remaining ethyl ether, then the temperature was decreased to 20C, 5mL 1N filtered calcium acetate was slowly added at constant speed at 20C. The addition process took around 30 minutes, and the temperature was kept at 20C. The mixture was stirred for 2 hours, then it was filtered, and the obtained solid was treated with 10mL 20C purified water, filtered and vacuum dried in sequence. As a result, 2.5g <strong>[287714-41-4]Rosuvastatin</strong> calcium was obtained.
  • 59
  • Nitro-Fosamprenavir [ No CAS ]
  • [ 62-54-4 ]
  • fosamprenavir calcium [ No CAS ]
YieldReaction ConditionsOperation in experiment
With ammonium formate In methanol; water 20 Preparation of Rod Like Amorphous Fosamprenavir Calcium from Methanol/Water Example 20 Preparation of Rod Like Amorphous Fosamprenavir Calcium from Methanol/Water Nitro-Fosamprenavir (2) (15.0 g; 24.5 mmol) and calcium acetate (4.24 g, 26.7 mmol) were suspended in methanol (180 ml) in a 500 ml round bottom flask. After 5 minutes ammonium formate (6.2 g; 97.5 mmol) and 10% Pd/C (960 mg, 3% w/w) were added and the reaction mixture was heated at 65° C. for 90 minutes. After the reaction was finished, the warm reaction mixture was filtered through Celite to remove the Pd/C catalyst and the filter cake was rinsed with methanol (2*30 ml). To the warm filtrate (50° C., 250 ml) water (62.5 ml) was added dropwise forming a suspension which was further stirred at room temperature overnight. The product (3, form I), a white solid, was filtered off and heated under vacuum at 45° C. for 3 hours and additionally 5 hours at 100° C. and 2 hours at 120° C.
With ammonium formate In methanol; ethanol; water 21 Preparation of Rod Like Amorphous Fosamprenavir Calcium from Methanol-Ethanol/Water Example 21 Preparation of Rod Like Amorphous Fosamprenavir Calcium from Methanol-Ethanol/Water Nitro-Fosamprenavir (2) (15.0 g; 24.5 mmol) and calcium acetate (4.24 g, 26.7 mmol) were suspended in a solvent mixture (methanol 70 ml and ethanol 110 ml) in a 500 ml round bottom flask. After 5 minutes, ammonium formate (6.2 g; 97.5 mmol) and 10% Pd/C (960 mg, 3% w/w) were added and the reaction mixture was heated at 65° C. for 90 minutes. After the reaction was finished, the warm reaction mixture was filtered through Celite to remove the Pd/C catalyst and the filter cake was rinsed with methanol (30 ml). To the warm filtrate (50° C., 210 ml) water (40 ml) was added dropwise. The resulting mixture was cooled to room temperature and a white suspension was obtained. The suspension was stirred at room temperature overnight. The product (3, form I), a white solid, was filtered off and heated under vacuum at 45° C. for 3 hours and additionally 5 hours at 100° C. and 2 hours at 120° C.
  • 60
  • [ 1332363-97-9 ]
  • [ 62-54-4 ]
  • 7-[4-(4-fluorophenyl)-6-isopropyl-2-(methanesulphonyl-methyl-amino)-pyrimidin-5-yl]-(3R,5S)-dihydroxy-hept-6-enoic acid calcium salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)-N,N-dimethylacetamide With hydrogenchloride In water at 15℃; for 2h; Stage #2: With potassium hydroxide In water at 35℃; for 70h; Stage #3: calcium acetate 10 10 g of ethylamine salt of Formula (8B2 Amine salt) and 90 mL acetonitrile in RBF at 25°C to 35°C. The reaction mixture was cooled to 0°C to 10°C. The reaction mixture was stirred and treated with 25 mL IN HCI and maintained for 2 hours at 20°C to 25°C. After the completion of the reaction on TLC, the reaction mixture was treated with 10% potassium hydroxide solution at 10°C to 15°C and maintained for 2 hours at 20°C to 25°C. After completion of the reaction as monitored by TLC, the reaction mixture was treated with IN HCI to get pH of 8 to 8.5 and charcoalized. The reaction mixture was filtered and washed with acetonitrile. The filtrate was extracted with mixture of toluene and ethyl acetate in the ratio of 7:3. at 25°C to 35°C. The solvents were distilled under vacuum at 35°C to 40°C to remove the traces of solvents and further treated with water to make up the volume upto 80 mL. The aqueous solution was treated with 3.2 g of calcium acetate solution in 15 mL of water and maintained for 1 hour at 20°C to 30°C. The solid thus obtained was filtered and washed with water. The solid was dried at 40°C under vacuum for 10 to 12 hours to obtain amorphous rosuvastatin calcium. Purity by HPLC > 99.0%.
  • 61
  • C2H7N*C25H32FN3O6S [ No CAS ]
  • [ 62-54-4 ]
  • 7-[4-(4-fluorophenyl)-6-isopropyl-2-(methanesulphonyl-methyl-amino)-pyrimidin-5-yl]-(3R,5S)-dihydroxy-hept-6-enoic acid calcium salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: C2H7N*C25H32FN3O6S With hydrogenchloride In water; acetonitrile at 20 - 25℃; for 2h; Stage #2: With potassium hydroxide In water; acetonitrile at 20 - 25℃; for 2h; Stage #3: calcium acetate 9 10 g of ethylamine salt of Formula (8B2 Amine salt) and 90 mL acetonitrile in RBF at 25°C to 35°C. The reaction mixture was cooled to 0°C to 10°C. The reaction mixture was stirred and treated with 25 mL IN HCI and maintained for 2 hours at 20°C to 25°C. After the completion of the reaction on TLC, the reaction mixture was treated with 10% potassium hydroxide solution at 10°C to 15°C and maintained for 2 hours at 20°C to 25°C. After completion of the reaction as monitored by TLC, the reaction mixture was treated with IN HCI to get pH of 8 to 8.5 and charcoalized. The reaction mixture was filtered and washed with acetonitrile. The filtrate was extracted with mixture of toluene and ethyl acetate in the ratio of 7:3. at 25°C to 35°C. The solvents were distilled under vacuum at 35°C to 40°C to remove the traces of solvents and further treated with water to make up the volume upto 80 mL. The aqueous solution was treated with 3.2 g of calcium acetate solution in 15 mL of water and maintained for 1 hour at 20°C to 30°C. The solid thus obtained was filtered and washed with water. The solid was dried at 40°C under vacuum for 10 to 12 hours to obtain amorphous rosuvastatin calcium. Purity by HPLC > 99.0%.
  • 62
  • [ 102-82-9 ]
  • [ 62-54-4 ]
  • [ 64-19-7 ]
  • [ 7204-64-0 ]
YieldReaction ConditionsOperation in experiment
With carbon dioxide In 2-Ethylhexyl alcohol; 2-ethylhexyl acetate; water; iso-butanol at 9℃; 4 Example 4; This example illustrates the effect of temperature on the percent organic acid salt conversion in the present innovation. In this example it is shown that decreasing the reaction temperature shifts the reaction equilibrium toward the acid amine complex product.Using the same apparatus as in Example 1, 2,100 ml of an aqueous feed of 21.15% by mass calcium acetate mono hydrate was combined with 2,271 ml of tributyl amine, 298 ml of 2-butanol, 1 ,632 ml of 2-Ethyl Hexanol, 276 ml of 2-Ethyl Hexyl Acetate, 180 ml of acetic acid and 48 ml of water and reacted with sparged carbon dioxide at 250 PSIG. After 60 minutes (sufficient time for the reaction to reach equilibrium), the reactor was cooled with an external jacket of ice water. Samples were taken at 35, 25, 15, 10 and 9 °C in approximately 15 minutes intervals between samples. The solvent and aqueous phases were analyzed for acetic acid using a calibrated GC with an FID detector. The aqueous phase was also analyzed for Ca2+ by Inductively Coupled Plasma Emission Spectroscopy at a contracted laboratory. Results are shown in Figure 6. As can be seen the acid salt conversion increase with lower temperatures.
  • 63
  • [ 102-82-9 ]
  • [ 62-54-4 ]
  • [ 4075-81-4 ]
  • [ 75775-31-4 ]
  • [ 7204-64-0 ]
YieldReaction ConditionsOperation in experiment
With carbon dioxide In 2-Ethylhexyl alcohol; 2-ethylhexyl acetate; water for 0.666667h; 5 Example 5; This example illustrates the affect of reaction residence time, % excess carbon dioxide, agitation power, different organic acids and synthetic vs. evaporated broth on a CCE continuous pilot unit simulating the first stage of a continuous counter-current multi-stage CCE and LLE system.With reference to Figure 7, a pilot unit was assembled to generate design data for a commercial counter-current multi-stage CCE and LLE process using the present invention. The unit was assembled such that an aqueous phase 10 containing synthetic or evaporated fermentation broth and a solvent phase 20 containing the solvent, amine and acid amine complex extracted by the solvent could be brought into contact and react with a gas phase containing carbon dioxide 30 to precipitate calcium carbonate and produce the acid amine complex. The aqueous stream 10 and solvent stream 20 were fed independently at an amine free S/F ratio of 0.8 via feed pumps 40 to a 2 gallon mixer/reactor (PARR reactor) 50 with a length to diameter ratio (L/D) of 2.875. One Ruchton turbine impeller 60 was placed directly above a sparge ring 70 at the bottom of the mixer/reactor 50 and two A- 315 impellers 60 were placed at standard impeller locations for gas dispersion. Carbon dioxide 30 was added to either the aqueous stream 10 or solvent stream 20 prior to the mixer/reactor 50 and brought into the bottom of the mixer/reactor 50 with the chosen liquid stream through the sparge ring 70. Agitator speed was variable from 150 RPM to 550 RPM. At the top of the reactor/mixer 50 was an outlet port that brought the slurry stream 60 through a back pressure control valve 70 that kept the system pressure constant at 250 PSI and directed the slurry stream 60 into a blow down tank 80. The blow down tank 80 was kept at atmospheric pressure and allowed for the dissociation of dissolved and excess carbon dioxide 90 from the slurry and exited through the top of the vessel. The slurry gravity drained from the blow down tank 80 into a vertical settler 100 with diameter of 4 inches and working height of 8 inches. In the vertical settler 100, the slurry separated into two liquid phases with the solids reporting to the aqueous phase. The extract (solvent phase) 110 was brought out of the top of the vertical settler 100. The raffmate and solids (aqueous phase) 120 was brought out from the bottom of the vertical settler 100 with a raffmate pump 130 that also controlled the liquid-liquid interface level. Samples were taken from the reactor/mixer 50 outlet every 30 minutes through a sample port 140 upstream from the back pressure control valve 70. The samples were immediately centrifuged and the solvent and aqueous phases analyzed for acid and amine using a calibrated GC with an FID detector. The aqueous phase was also analyzed for Ca by Inductively Coupled Plasma Emission Spectroscopy at a contracted laboratory. Results for several runs are shown in Table 3.
  • 64
  • [ 628-63-7 ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
With water; calcium hydroxide at 80℃; for 1h; 14 Example 14; When the bulk solvent used in this innovation contains an alcohol, it is likely that small amounts of the alcohol in the solvent will react with the organic acid to make an ester. Because alcohols have higher extraction coefficients for the acid/amine complex than their corresponding ester, it is desired to keep a steady state composition of the solvent where the wt% of the alcohol component is greater than the wt% of the ester component. This can be done by taking a small split stream from the solvent leaving the acid recovery section and saponifying or hydrolyzing the ester component in the solvent to produce the acid and the alcohol. The split stream can then be recombined with the rest of the solvent.This example illustrates the saponifaction of an ester to its respective alcohol and carboxylic acid. In this example pentyl acetate (PeAc) is saponified to pentanol (PeOH) and an acetic acid salt.202ml of an aqueous 15 wt% solution of sodium hydroxide (NaOH), is added to a jacketed reactor made by ChemGlass and combined with 214ml of pentanol and heated to 80C. To this mixture, PeAc is added to a molar ratio of 1:1.1 PeAcrNAOH and the reactor is sampled at various time intervals. Samples are analyzed for PeAc by gas chromatography. The same experiment is repeated another two times, the first time using potassium hydroxide (KOH) as the base and the second time using calcium hydroxide as the base. The quantities of base, PeOH and PeAc were the same as the first experiment. Figure 15 shows the change in wt% PeAc vs. time for the three experiments.
  • 65
  • tetrabutoxytitanium [ No CAS ]
  • zirconium(IV) tetraisopropoxide [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • (Ba0.9Ca0.1)(Ti0.9Zr0.1)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
With 2-methoxy-ethanol In acetic acid at 60 - 700℃; Synthesis of the films of BCZT relies on the preparation of stable precursor sol. Precursor sol of BCZT was prepared by the sol-gel method. Barium acetate (Ba(CH3COO)2), calcium acetate (Ca(CH3COO)2), zirconium (IV) isopropoxide (Zr(OC3H7)4) and terabutyl titanate (Ti(OC4H9)4) were used as starting materials. Glacial acetic acid (CH3COOH) and ethylene glycol monomethyl ether (HOCH2CH2OCH3) were used as a solvent. According to the stoichiometric ratio of (Ba0.9Ca0.1)(Ti0.9Zr0.1)O3, firstly, terabutyl titanate was dissolved in the ethylene glycol monomethyl. Zirconium (IV) isopropoxide was then added at 60 °C with continuous stirring for 30 min. A stoichiometric amount of the barium acetate and calcium acetate were dissolved in glacial acetic acid, stirred at 60 °C until dissolved completely. The above two solutions were mixed with continuous stirring at 60 °C for 2 h to obtain a stable precursor sol of BCZT. The precursor sols of BCZT were dried at 100 °C for 12 h to prepare BCZT powders for the XRD analysis. In order to investigate the effects of annealing processes on the structure and properties of materials, the films were prepared under three different annealing processes.
  • 66
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • [ 792848-15-8 ]
YieldReaction ConditionsOperation in experiment
With sodium dodecyl-sulfate; urea; 1,3,5-trimethyl-benzene at 120℃; for 1h; Autoclave; High pressure; 2.2 Methods In a typical preparation of CaCO3 crystals, an aqueous solution contained 50mM calcium acetate, 0.25mM urea, and 5.0mM SDS was prepared in a beaker. The pH value of the solution was 8.0. Different amounts of TMB were added into the beaker, in which the molar ratio of TMB to SDS was 0/1, 1/20, 1/10, 1/5, 1/2, 1/1, and 10/1, respectively. The solution was stirred with a magnetic blender for about 15-20min. 80ml of the solution was transferred into a Teflon-lined stainless-steel autoclave (100ml). The autoclave was placed in an oven, which the temperature of the oven was controlled at 90°C and 120°C for different times, respectively. After the hydrothermal treatment, the autoclave was pulled out the oven to cool down in air to room temperature. The resulting solid sample was washed with water and alcohol several times, and dried for more than 24h at room temperature in vacuum.
  • 67
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • [ 792848-15-8 ]
  • [ 792848-15-8 ]
YieldReaction ConditionsOperation in experiment
With sodium dodecyl-sulfate; urea; 1,3,5-trimethyl-benzene at 90℃; for 6h; Autoclave; High pressure; 2.2 Methods In a typical preparation of CaCO3 crystals, an aqueous solution contained 50mM calcium acetate, 0.25mM urea, and 5.0mM SDS was prepared in a beaker. The pH value of the solution was 8.0. Different amounts of TMB were added into the beaker, in which the molar ratio of TMB to SDS was 0/1, 1/20, 1/10, 1/5, 1/2, 1/1, and 10/1, respectively. The solution was stirred with a magnetic blender for about 15-20min. 80ml of the solution was transferred into a Teflon-lined stainless-steel autoclave (100ml). The autoclave was placed in an oven, which the temperature of the oven was controlled at 90°C and 120°C for different times, respectively. After the hydrothermal treatment, the autoclave was pulled out the oven to cool down in air to room temperature. The resulting solid sample was washed with water and alcohol several times, and dried for more than 24h at room temperature in vacuum.
  • 68
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • [ 792848-15-8 ]
  • [ 792848-15-8 ]
YieldReaction ConditionsOperation in experiment
With sodium dodecyl-sulfate; urea; 1,3,5-trimethyl-benzene at 90℃; for 24h; Autoclave; High pressure; 2.2 Methods In a typical preparation of CaCO3 crystals, an aqueous solution contained 50mM calcium acetate, 0.25mM urea, and 5.0mM SDS was prepared in a beaker. The pH value of the solution was 8.0. Different amounts of TMB were added into the beaker, in which the molar ratio of TMB to SDS was 0/1, 1/20, 1/10, 1/5, 1/2, 1/1, and 10/1, respectively. The solution was stirred with a magnetic blender for about 15-20min. 80ml of the solution was transferred into a Teflon-lined stainless-steel autoclave (100ml). The autoclave was placed in an oven, which the temperature of the oven was controlled at 90°C and 120°C for different times, respectively. After the hydrothermal treatment, the autoclave was pulled out the oven to cool down in air to room temperature. The resulting solid sample was washed with water and alcohol several times, and dried for more than 24h at room temperature in vacuum.
  • 69
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • [ 792848-15-8 ]
YieldReaction ConditionsOperation in experiment
With sodium dodecyl-sulfate; urea; 1,3,5-trimethyl-benzene at 90℃; for 24h; Autoclave; High pressure; 2.2 Methods In a typical preparation of CaCO3 crystals, an aqueous solution contained 50mM calcium acetate, 0.25mM urea, and 5.0mM SDS was prepared in a beaker. The pH value of the solution was 8.0. Different amounts of TMB were added into the beaker, in which the molar ratio of TMB to SDS was 0/1, 1/20, 1/10, 1/5, 1/2, 1/1, and 10/1, respectively. The solution was stirred with a magnetic blender for about 15-20min. 80ml of the solution was transferred into a Teflon-lined stainless-steel autoclave (100ml). The autoclave was placed in an oven, which the temperature of the oven was controlled at 90°C and 120°C for different times, respectively. After the hydrothermal treatment, the autoclave was pulled out the oven to cool down in air to room temperature. The resulting solid sample was washed with water and alcohol several times, and dried for more than 24h at room temperature in vacuum.
  • 70
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • [ 546-68-9 ]
  • [ 62-54-4 ]
  • La0.8Ca0.2TiO(3-x) [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: lanthanum(III) nitrate hexahydrate; titanium(IV)isopropoxide; calcium acetate With citric acid In water at 60℃; for 8h; Stage #2: at 120℃; for 24h; Stage #3: at 800℃; for 2h; Precursors were dissolved in 50 mL distilled water. After the formation of the clear solution 26 mmol citric acid and 5 mmol of polyethylene glycol were added and the solution was heated to 60 C with continuous stirring for 8 h to obtain gel. Later the gel was placed in an oven for 24 h at 120 C till it dried to become a brown porous solid. Further, the dried gel was calcined at 800 C for 2 h
  • 71
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • titanium tetraisopropoxide [ No CAS ]
  • [ 62-54-4 ]
  • La0.8Ca0.2TiO(3-x) [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: lanthanum(III) nitrate hexahydrate; titanium tetraisopropoxide; calcium acetate With citric acid In water at 60℃; for 8h; Stage #2: at 800℃; for 2h; Calcination; 2. Experimental details General procedure: High purity (99.9%) Sigma-Aldrich chemicals La(NO3)3*6H2O, Ba(C2H3O2)2, Sr(C2H3O2)2, Ca(C2H3O2)2, and C12H28O4Ti were used as precursors for the synthesis of undoped, A-site doped (La0.8A0.2TiO3d, A = Ba, Sr, Ca) lanthanum titanate(LaTiO(3-x)) perovskites using wet chemical method (i.e., citric acid sol-gel method). The undoped LaTiO(3-x) gel was synthesized using 4.5 mmol of La(NO3)3*6H2O, 4.5 mmol of C12H28O4Ti and the precursors were dissolved in 50 mL distilled water.After the formation of the clear solution 26 mmol citric acid and 5 mmol of polyethylene glycol were added and the solution was heated to 60° C with continuous stirring for 8 h to obtain gel. Later the gel was placed in an oven for 24 h at 120° C till it dried to become a brown porous solid. Similar method was followed for the A-site doped perovskites. Further, the dried gel was calcined at 800° C for 2 h.
  • 72
  • silica-alumina [ No CAS ]
  • [ 62-54-4 ]
  • None [ No CAS ]
YieldReaction ConditionsOperation in experiment
1.845 g In water at 600℃; for 5h; 21 After 2.006 g of HZSM-5 (SiO2/Al2O3=280) was impregnated with a solution in which 0.053 g of calcium acetate monohydrate was dissolved in 20.189 g of deionized water, and the resultant was dried and calcinated at 600° C. for 5 hours, thereby obtaining 1.845 g of a cracking catalyst 7. From the result of the ICP analysis, the oxide content (molar ratio) of the obtained cracking catalyst 7 was SiO2/Al2O3/CaO=297/1.00/2.28.
  • 73
  • [ 17754-90-4 ]
  • [ 62-54-4 ]
  • [ 18514-52-8 ]
  • C26H28CaN6O2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% In ethanol at 70℃; for 12h;
  • 74
  • tetrabutoxytitanium [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • erbium(III) nitrate [ No CAS ]
  • None [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: tetrabutoxytitanium; calcium acetate; barium(II) acetate; erbium(III) nitrate In ethanol; water; acetic acid at 49.84 - 59.84℃; for 1h; Stage #2: at 899.84 - 1399.84℃; for 7h; 2 Methods A 1mol% Er3+ doped BCT ceramic was prepared by the sol-gel method. Barium acetate (Ba(CH3COO)2), calcium acetate (Ca(CH3COO)2), tetrabutyl titanate (TiC16H36O4), and erbium nitrate solution (Er(NO3)3) were used as raw materials. Absolute ethyl alcohol and glacial acetic acid were used as solvents. Ba(CH3COO)2, Ca(CH3COO)2, and Er(NO3)3 were first dissolved in a solution of glacial acetic acid and deionized water, according to the stoichiometric ratios. The solution was stirred for 0.5hat 323K, and then, tetrabutyl titanate was dissolved in a separate solution of absolute ethyl alcohol and glacial acetic acid. While all the solutions were cooled to room temperature, the former solution was added dropwise to the latter. The resulting solution was stirred at 333K. After 0.5h, a clear gel was formed. This precursor was dried in an oven at 353K for 12h and then calcined at 1173K for 3h. The resulting powders were pressed into disk pellets and sintered at 1673K for 4h. The samples were coated with silver paste and fired at 823K for 0.5h for ferroelectricity and piezoelectricity testing. Then, the sample was polished for optical tests.
  • 75
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.93Ca0.07(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 76
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.98Ca0.02(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 77
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.97Ca0.03(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 78
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.96Ca0.04(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 79
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.95Ca0.05(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 80
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • titanium(IV) oxide [ No CAS ]
  • tin(IV) oxide [ No CAS ]
  • Ba0.94Ca0.06(Ti0.91Sn0.09)O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate; titanium(IV) oxide; tin(IV) oxide With citric acid In water at 80℃; for 10h; Stage #2: at 250 - 1250℃; for 27h; Calcination; Stage #3: air at 750 - 1400℃; for 7h; 2.1 Ceramic sample preparation General procedure: BCTS powders were prepared by the conventional solid-state reaction combined with a gel precursor mixing method. First, analytically pure metal acetate Ba(CH3COO)2 (99.0%) and Ca(CH3COO)2 (98.0%) were dissolved in distilled water and mixed under constant stirring, followed by adding a certain amount of TiO2 (99.5%), SnO2 (99.5%) and 16-20g citric acid monohydrate (C6H8O7·H2O). Then, the solution was kept at 80°C for 10h until the gelation process completed. After that, the gel precursor was calcined at 250°C for 6h, followed by an initial calcination at 750°C for 5h and a second calcination at 1200°C for 8h in air atmosphere. The obtained powders were mixed by ball milling in alcohol using zirconia balls for 12h. After the ball milling, the powders were calcined again at 1250°C for a further 8h. Finally, the calcined powders were ball-milled one more time for 12h and then dried and sieved, followed by the addition of polyvinyl alcohol (PVA) as a binder. The resulting powders were then sieved, granulated, and pressed into disk shaped samples with a diameter of 10mm and a thickness of ∼1mm. All the samples were sintered at 1400°C for 2h in air after burning out the PVA binder at 750°C for 5h. By the improved method, uniformly mixed raw materials and ceramics with relatively uniform particle size and sharp grain boundaries were easily obtained.
  • 81
  • [ 472967-95-6 ]
  • [ 62-54-4 ]
  • calcium (3S,5S)-7-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-(phenylcarbamoyl)pyrrol-1-yl]-3,5-dihydroxyheptanoate [ No CAS ]
YieldReaction ConditionsOperation in experiment
12.7 g Stage #1: tert-butyl (4S,6S)-6-{2-[2-(4-fluorophenyl)-5-isopropyl-3-phenyl-4-(phenylcarbamoyl)pyrrol-1-yl]ethyl}-2,2-dimethyl-1,3-dioxane-4-acetate With hydrogenchloride In methanol; water at 35℃; for 5h; Stage #2: calcium acetate In methanol; water at 30℃; for 16h; 1.4 Step 4: (3S, 5S) - statins atorvastatin calcium prepared (3S, 5S) -termade obtained by the above procedure,Into a 500 mL round bottom flask.To this was added 135 mL of methanol,27g1M hydrochloric acid (take commercially available pure concentrated hydrochloric acid,Diluted to 12 times the original volume),Heated at 35 ° C for about 3 hours,Heating to 2 hours or so when the solution from the turbidity to clarify.Add 1N sodium oxide to adjust the pH to 9-10 (take 4g sodium hydroxide,Dissolved in water diluted to about 100mL, 1N sodium hydroxide aqueous solution).The pH was maintained at about 9-10 with 1N sodium hydroxide solution,50-55 & lt; 0 & gt; C continue to maintain pH and react for 2 hours,Until the reaction is complete.The reaction solution was poured into a solution of 4.5 g of calcium acetate monohydrate 215 mL of water and heated to about 30 ° C overnight for about 16 hours.The precipitate was collected by filtration,Room temperature drying after drying about 15g,To this was added 150 mL of ethyl acetate,Heated at 40 ° C for 30 minutes,So that most of the solid dissolved.Filter to remove a small amount of insoluble matter,To this was added 150 mL of n-hexane with stirring,A large amount of white solid precipitated in the solution.Stirred at room temperature for 2 hours,The precipitate was collected by filtration,Dried at 60-70 & lt; 0 & gt; C overnight,The white solid was (3S, 5S) -itocortastatin calcium,Weight 12.7g. HPLC found that its purity is greater than 95%.
  • 82
  • [ 67-66-3 ]
  • C32H32N4O10 [ No CAS ]
  • [ 62-54-4 ]
  • [ 5970-45-6 ]
  • [Zn2(L)Ca(OAc)2]*CHCl3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
45.6% In water 2.3.2 Syntheses of the heterotrinuclear complexes A solution of Zn(OAc)2·2H2O (6.58mg, 0.03mmol) in methanol (1mL) and Ca(OAc)2 (1.58mg, 0.01mmol) in water/methanol (1:3, 2mL) were added to a solution of H4L (6.32mg, 0.01mmol) in chloroform (3mL), and the resulting solution was concentrated to dryness. The solid was redissolved in chloroform/methanol (1:1, 6mL). The mixture was filtered and the filtrate was allowed to stand at room temperature for several weeks, giving yellow crystals of complex 2. Complexes 3 and 4 were prepared by a similar procedure as for complex 2. Complex 2, yellow crystals, Yield: 4.73mg (45.6%). Anal. Calc. for C37H35CaCl3N4O14Zn2: C, 42.86; H, 3.40; N, 5.40. Found: C, 42.79; H, 3.23; N, 5.27%. IR (KBr; cm-1): 1610 [ν(C=N)], 1238 [ν(Ar-O)]. UV-vis [in chloroform/methanol (1:1)], λmax (nm) [3.3×10-5 M)]: 280, 370, 396, 416.
  • 83
  • C32H32N4O10 [ No CAS ]
  • [ 62-54-4 ]
  • [ 6147-53-1 ]
  • C36H34CaCo2N4O14 [ No CAS ]
YieldReaction ConditionsOperation in experiment
44.65% In methanol; water at 20℃; General procedure: A solution of Co(OAc)2·4H2O (9.96 mg, 0.040 mmol) in methanol (2 mL) and Ca(OAc)2 (3.16 mg, 0.020 mmol) in water/methanol (1:3, 2 mL) were added to a solution of H4L (12.64 mg, 0.020 mmol) in chloroform (4 mL), and the resulting solution was evaporated to dryness, after which the solid was redissolved in chloroform/methanol (1:1, 8 mL). The mixture was filtered and the filtrate was allowed to stand at room temperature for several weeks to obtain complex 2. Complexes 3 and 4 were prepared by a similar procedure as for complex 2, however, complex 4 was prepared using ethanol as the solvent instead of methanol that was used for complex 2. Complex 2, dark yellow crystals, yield: 44.65%. Elemental analysis, Anal. Calc. for C36H34CaN4O14Co2: C, 47.80; H, 3.79; N, 6.19; Co, 13.03; Ca, 4.43. Found: C, 47.49; H, 3.23; N, 6.42; Co, 12.89; Ca, 4.20%. IR (KBr; cm-1): 1596 [ν(C=N)], 1250 [ν(Ar-O)], 3417 [ν(O-H)]. UV-Vis [in methanol/chloroform (1:1)], λmax (nm) [2.5 * 10-5 M]: 290, 373, 415.
  • 84
  • sodium dihydrogenphosphate dihydrate [ No CAS ]
  • [ 62-54-4 ]
  • octacalcium phosphate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water at 70℃; for 2h; 1 Production Example 1: Preparation of OCP Production Example 1: Preparation of OCP (0078) Liquid 1 and liquid 2 for preparation of OCP were prepared in the following manner. Sodium dihydrogen phosphate dihydrate (31.2 g) was dissolved in 2,500 g of distilled water to prepare liquid 1. Calcium acetate monohydrate (35.2 g) was dissolved in 2,500 g of distilled water to prepare liquid 2. Liquid 1 was placed in a separable flask, and heated to 70° C. using a mantle heater. While stirring liquid 1 at a rate of 250 rpm using a stirrer (MAZELA Z, produced by Tokyo Rikakikai Co., Ltd.) to which a stirring blade (blade diameter: 12 cm) was attached, liquid 2 was dropped at a rate of about 28 mL/min. After the completion of dropping, the mixture of liquid 1 and liquid 2 was further stirred at 70° C. at 250 rpm for 2 hours. (0079) The precipitate produced in the above mixture was filtered through a membrane filter (pore size: 3 μm; A300A293C, produced by Advantec Toyo Kaisha, Ltd.), and collected. The collected precipitate was dispersed in 1,500 mL of distilled water, and washed by stirring for 15 minutes. The process of filtering and washing was further repeated 3 times. The washed precipitate was dried in a constant temperature dryer at 30° C. for 24 hours. After the dried precipitate was ground with an electric mill, the ground product was classified using a sieve to a particle size of 300 to 500 μm. Thus, a powder was obtained. Finally, the obtained powder was subjected to dry sterilization at 120° C. for 2 hours, thereby obtaining OCP.
  • 85
  • [ 15722-48-2 ]
  • [ 62-54-4 ]
  • C14H6N2O6(4-)*Ca(2+)*2H(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With water at 90℃; Sonication; 1 In an alternative synthesis, Ca(OAc)2-2H20 (27.7 mg, 0.160 mmol) was dissolved in 1 mL of water and olsalazine acid (22.7 mg, 0.0750 mmol) was suspended in 4 mL of water with sonication. The combined solutions were then sonicated together and left to heat at 90 °C to produce yellow or red crystals depending on size. A shorter sonication time (1 min) correlated with larger crystals, while longer sonication times (> 5 min) produced a more uniform distribution of crystals by size.
  • 86
  • [ 7446-08-4 ]
  • [ 62-54-4 ]
  • [ 10108-64-2 ]
  • Ca0.7Cd2.3(SeO3)3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
86% With potassium nitrate In water at 210℃; for 96h; High pressure; Autoclave;
  • 87
  • [ 142-71-2 ]
  • [ 62-54-4 ]
  • titanium(IV) oxide [ No CAS ]
  • calcium copper titanate [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: copper diacetate; calcium acetate; titanium(IV) oxide With potassium chloride; sodium chloride for 0.416667h; Milling; Stage #2: at 800℃; for 1h; Calcination; 2. Experimental procedure The CCTO were prepared using a simple molten salt synthesis method. A detailed synthesis procedure has been extensively described in our earlier work [41]. In brief calcium acetate, copper acetate, titanium dioxide, NaCl, and KCl were taken in a molar ratio of1:3:4:40:40 and mixed in a mortar for 25 min. The mixture was then heated in an air furnace at 800 °C for three different holding time (30 min, 1 h and 5 h).
  • 88
  • [ 62-54-4 ]
  • magnesium acetate [ No CAS ]
  • CaMg<SUB>2</SUB>(acetate)<SUB>6</SUB> [ No CAS ]
YieldReaction ConditionsOperation in experiment
With acetic acid In water at 80℃; C) Calcium magnesium acetate crystals from mixtures of calciumacetate monohydrate, Ca(OAc)2·H2O and magnesium acetate tetrahydrate,Mg(OAc)2·4H2O The process followed the procedure as outlined above, for CMAcrystals from commercial CMA samples. Ca(OAc)2·H2O andMg(OAc)2·4H2O were mixed in a 1:2 mol ratio. 500 mg quantitiesof the mixture were suspended in 1 mL glacial acetic acid andheated to ca 80 °C in open vessels (5 mL scintillation vials withloosely screwed on caps) upon which all material completelydissolved. Water and acetic acid were completely boiled off. Theprocess was repeated twice to assure that all water was completelyremoved from the sample. Recrystallization from acetic acid (ca. 1mL) by slow cooling from 80 °C to room temperature yielded singlecrystals of CMA. Crystals were isolated from remaining glacial acetic acid, washed with acetone, dried in air and analyzed by singlecrystal X-ray diffraction unit cell determination and powder X-raydiffraction.
  • 89
  • [ 64-19-7 ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
100% With calcium carbonate In water 4.1.1. Calcium acetate monohydrate, Ca(OAc)2·H2O Calcium acetate was prepared from calcium carbonate and dilutedacetic acid. The solubility of calcium acetate decreases with temperature,thus no crystalline material can be obtained by cooling ofsaturated solutions [36]. Calcium acetate monohydrate was insteadisolated by salting out with acetone from the reaction mixture,following the procedure described by Panzer [29]. Acetone was slowlyadded to the vigorously stirred solution to form a fine precipitate.When no more solid formed the precipitate was filtered off withsuction. The filter cake was washed with copious amounts of acetone,isolated and suspended again in acetone with vigorous stirring, and thesolid again filtered off with suction. The process was repeated twiceuntil the filter cake was essentially odorless (no acetic acid smell). Thesolid was dried in air for several days with intermediate breaking upand grinding, and analyzed by powder X-ray diffraction. Rietveldrefinement yielded one of the triclinic polymorphs of calcium acetatemonohydrate [16] with lattice constants a = 6.755, b = 11.103, c =11.801 Å, α = 116.41, β = 92.40, γ = 97.52° as the only crystallinecomponent, with no indication of the other reported polymorph[37,38] being present (see SI for details, Fig. S1). The material wasstored in a closed container until further use. The yield was essentiallyquantitative.
With calcium hydroxide
  • 90
  • methyl (3R,5S,E)-7-(2-(1-chloro-N-methylmethylsulfonylamino)-4-(4-fluorophenyl)-6-isopropylpyrimidin-5-yl)-3,5-dihydroxyhept-6-enoate [ No CAS ]
  • [ 62-54-4 ]
  • calcium (3R,5S,E)-7-(2-(1-chloro-N-methylmethylsulfonylamino)-4-(4-fluorophenyl)-6-isopropylpyrimidin-5-yl)-3,5-dihydroxyhept-6-enoate [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% Stage #1: methyl (3R,5S,E)-7-(2-(1-chloro-N-methylmethylsulfonylamino)-4-(4-fluorophenyl)-6-isopropylpyrimidin-5-yl)-3,5-dihydroxyhept-6-enoate With sodium hydroxide In acetonitrile at 60℃; for 1h; Stage #2: calcium acetate In acetonitrile 1 Add to the reaction flask containing acetonitrile (20ml) (3R,5S,E)-7-(2-((1-chloro-N-methylmethyl)sulfonamido)-4-(4-fluorophenyl)-6-isopropylpyrimidine-5 -yl)-3,5-dihydroxyhept-2-enehept-6-enoic acidMethyl ester (130mg),Warming up to 60 ° C,Slowly add sodium hydroxide solution (20ml, 0.1N).The reaction was stirred for 1 h.Distilling off acetonitrile under reduced pressure,Water was then added to the residue and glacial acetic acid solution was added to adjust the pH.Stir and let go layering,The aqueous layer was washed with tert-butyl methyl ether (40 mL).The organic layers were combined, and a solution of calcium acetate (20 ml) was added dropwise and stirred.Filtration, the solid is beaten with water and then filtered.(3R, 5S, E)-7-(2-((1-Chloro-N-methylmethyl)sulfonylamino)-4-(4-fluorophenyl)-6-isopropylpyrimidin-5-yl)-3,5-dihydroxyheptane- 6-enoate calcium salt (241 mg) in a yield of 95%.
  • 91
  • [ 62-54-4 ]
  • [ 125971-95-1 ]
  • [ 134523-03-8 ]
YieldReaction ConditionsOperation in experiment
With hydrogenchloride In methanol Heating; 4 10 g of the atorvastatin calcium condensate containing the impurity A and 100 mL of methanol were mixed, and the pH was adjusted to 2 with dilute hydrochloric acid, and the reaction was stirred with heating, and the progress of the reaction was monitored by HPLC.After the reaction was completed, an aqueous sodium hydroxide solution was added to the above reaction solution to adjust the pH to 13,The reaction was heated and stirred until the end of the reaction. A calcium acetate aqueous solution (2.0 g of calcium acetate, 100.0 g of 7JO was added dropwise to the reaction solution, and the reaction was terminated by HPLC to obtain atorvastatin calcium. After detection, the impurity atorvastatin calcium was detected. The content of the dimer was 0.36%.
  • 92
  • C2H8N4O4Pt [ No CAS ]
  • [ 62-54-4 ]
  • tetraammineplatin acetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
92.84% With acetic acid In water for 0.5h; 1-3 A preparation method of tetraammineplatinum (II) acetate, comprising the following steps: Weigh 140g (1.555mol) of oxalic acid into a 5000mL beaker.Add 1000 mL of deionized water and stir to dissolve.Then slowly add 200 g (0.451 mol) of ammonium chloroplatinate solid in portions.The reaction was stirred at 50 ° C for 1 h, the stirring was stopped, and the mixture was allowed to stand for 10 min to filter.A solution of diammonium oxalate (II) (143.0 g) was obtained.Slowly add 785 mL (715 g) of ammonia water to the diammonium oxalate (II) solution.Control temperature is 50~60 °C,Reaction for 3h,Stop heating, cool to room temperature, and dissolve 190g of calcium acetate in 600mLDeionized water, dissolved, and then slowly added calcium acetate solution to tetraammine oxalate (158.3g) solution, not to generateAfter precipitation, 50 mL of acetic acid was added, stirring was continued for 0.5 h, and allowed to stand for 30 min to obtain tetraammineplatin acetate solution and white precipitated grass.Calcium acid, filtered, and washed twice with appropriate amount of deionized water. The filtrate and washing water were combined and concentrated under reduced pressure at 80 ° C to obtain 180 mL of concentratedLiquid shrinkage, add 10mL acetic acid, then add the concentrated solution with acetic acid to 3000mL acetone solution, precipitate white knotThe crystals were filtered, washed with methanol and dried at 50 to 80 ° C for 2 h to obtain 159.6 g of tetraammineplatin acetate. The yield was 92.84%.
  • 93
  • ammonium dihydrogen phosphate [ No CAS ]
  • [ 62-54-4 ]
  • calcium hydroxyapatite [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: ammonium dihydrogen phosphate; calcium acetate In acetone at 600℃; for 5h; Stage #2: at 800℃; for 8h; Ca10(PO4)6(OH)2 samples were synthesized by the conventional solidstatemethod. The starting materials, Ca(AcO)2H2O (5.285 g) andNH4H2PO4 (2.066 g), were carefully mixed in agate mortar with acetone(30 ml) for ~20 min until the evaporation of solvent. The Ca:P molarratio of 1.67 was always maintained in the synthesis. The powders werepreheated at 600°C for 5 h with a heating rate of 1 K min-1. The intermediatepowders were annealed at three different temperatures (800, 900and 1000°C) for 8 h with a heating rate of 2 K min-1. The obtainedproducts were characterized by powder X-ray diffraction (XRD) analysisusing a Rigaku MiniFlex II diffractometer working in Bragg-Brentano(q/2q) geometry. SEM images were obtained on a Hitachi SU-70 microscope.IR spectra were recorded using a PerkinElmer Frontier FTIRspectrometer.
  • 94
  • [ 1021497-97-1 ]
  • [ 62-54-4 ]
  • C20H17BrN3O3S(1-)*Ca(2+)*C2H3O2(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
In water at 20 - 50℃; for 120h; 1; 3 EXAMPLE 1 : 4 -(2-((4-bromophenyl)thio)acetamido)-1-phenethyl-1 H-pyrazole-3- carboxylic acid potassium salt General procedure: Ca. 25mg of the compound 1 (KM-00819) was weighed into a 2 mL HPLC vial prior to the addition of 1500pL. To the resulting slurries was added 1.1 eq of potassium hydroxide in 60 ul in water (to 1 M concentration). The sample was placed on to a maturation cycle for 5 days using an 8 hour cycle (4 hours at RT followed by 4 hours at 50°C). Post-maturation the sample was re-examined and then filtered and dried in vacuo.
  • 95
  • [ 62-54-4 ]
  • [ 75-07-0 ]
  • [ 78-98-8 ]
  • [ 25566-16-9 ]
YieldReaction ConditionsOperation in experiment
With manganese; sulfuric acid; tetra-(n-butyl)ammonium iodide; iron; zinc In water at 35℃; for 2h; 3.2-3.3; 1-7 (2) Preparation of 3,4-dihydroxy-2,5-hexanedione solution: in a funnel equipped with a thermometer, a constant-pressure dropping funnel,In a four-necked flask with a mechanical stirring device and air duct, add 50 mL of pure water, 15 g of calcium acetate and 1 g of tetrabutylammonium iodide, stir and dissolve, add 5 g of zinc powder,2g of iron powder and 1g of manganese powder, 40 mL of 25% aqueous solution of acetaldehyde and 15 mL of diluted sulfuric acid were added dropwise, and the temperature was controlled at 20 ° C during the dropwise addition.5g of zinc powder, 2g of iron powder and 1g of manganese powder were added, and at the same time 40mL of 25% aqueous solution of pyruvaldehyde and 15mL of diluted sulfuric acid were added dropwise.After the dropwise addition, the temperature was raised to 35 ° C. and the temperature was maintained for 2 hours to obtain a 3,4-dihydroxy-2,5-hexanedione solution. The yield of 3,4-dihydroxy-2,5-hexanedione was 87.4%. (3) Purification of 3,4-dihydroxy-2,5-hexanedione: Add 2g yuanming powder and 3g sodium chloride to 3,4-dihydroxy-2,5-hexanedione solution, and centrifuge Separation, separated zinc powder,Iron powder and manganese powder are returned to step (2) for reuse, and the separated liquid phase is added with ethyl acetate extractant for extraction.The extraction is performed in a secondary extraction tower to obtain an extraction solution, followed by evaporation and concentration of the oil phase.Recover ethyl acetate and distilled water to obtain an extract concentrate; after freeze crystallization,3,4-dihydroxy-2,5-hexanedione mother liquor and purified 3,4-dihydroxy-2,5-hexanedione, 3,4-dihydroxy-2,5-hexanedione were obtained by centrifugation The purity of the ketone is 99.98%.
  • 96
  • iron(II) chloride tetrahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 62-54-4 ]
  • [ 64-19-7 ]
  • μ3-oxo-hexa(acetato)tri(aqua)iron(II)diiron(III) [ No CAS ]
YieldReaction ConditionsOperation in experiment
72.1% at 69.84℃; for 6h;
  • 97
  • tetrabutoxytitanium [ No CAS ]
  • Iron(III) nitrate nonahydrate [ No CAS ]
  • bismuth (III) nitrate pentahydrate [ No CAS ]
  • [ 62-54-4 ]
  • Bi0.8Ca0.2Fe0.8Ti0.2O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
With acetic acid at 500℃; for 1h; Irradiation; 2. Experimental The BF-20CT nanocrystalline powder was prepared by the sol-gelroute [28,34]. Bi(NO3)35H2O (HiMedia, 98%), Fe(NO3)39H2O(HiMedia, 98%), Ca(CH3COO)2H2O (HiMedia, 99.0%), and C16H36O4Ti(Sigma-Aldrich, 97%) were used as the starting precursors, while aceticacid (Sigma-Aldrich, 99.7%) and 2-methoxyethanol (Sigma-Aldrich,99%) were used as solvents to prepare the precursor solution. The solutionwas placed under IR Lamp to evaporate the solvents. The driedprecursor powder was crushed and given the heat treatment at 500 C,650 C, 800 C and 950 C (sample named as S1, S2, S3, and S4,respectively) at a heating rate of 2 C/min for 1 h. The phase purity andcrystal structure at room temperature of all samples were inspected byX-ray diffractometer (XRD, Rigaku Miniflex 600) operated at 40 kV, 15mA with CuKα radiation (λ = 1.54 Å). The XRD data were recorded usinga 0.02 step size with a scan rate of 1 per minute over the 2θ range of20-120. The crystallite sizes (DXRD) were calculated by the Scherrer’sformula [28,34]. The Fullprof suite software was used to perform thestructural analysis by Rietveld refinement [35,36]. The background wasconsidered with a linear interpolation method. The Pseudo-Voigt functionwas used to define the peak shape. Zero correction parameters,lattice parameters, and background were refined simultaneously andlater, the half-width parameters (u, v, and w) were refined. The atomicpositions were added consecutively, starting with the heavier atoms tothe refinement after getting convergence. Thermal displacement parameterswere refined, and the anisotropic peak broadening wasconsidered. Transmission electron microscopy (TEM, JEOL 2100 F)operated at 200 kV was performed to study the size, morphology, andmicrostructure of the samples. The sample was well dispersed in ethanolfor 4 h using ultra-sonication before finally drop cast to thecarbon-coated grid. Energy-dispersive X-ray spectroscopy (EDX)attached with a scanning electron microscope (SEM, Zeiss EVO40) wasused for compositional analysis. The magnetic measurements wereperformed on a physical property measurement system (PPMS, CryogenicsLimited, USA).
  • 98
  • tetrabutoxytitanium [ No CAS ]
  • [ 62-54-4 ]
  • [ 6046-93-1 ]
  • calcium copper titanate [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; copper(II) acetate monohydrate In water at 85℃; for 1h; Stage #2: tetrabutoxytitanium at 85℃; for 1h; Stage #3: air at 1100℃; The precursor of ceramic powder of CCTO wassynthesized by liquid-phase method in acetic acidmedium. Initial reagents used were Ca(OH)2,Cu(CH3COO)2 · H2O, Ti(C4H9O)4 (in stoichiometricratio CaO : CuO : TiO2 = 1 : 3 : 4), and glacial aceticacid (all chemicals from SIGMA-Aldrich). Synthesisprocedure consisted in the preparation of aqueoussolution of Cu(CH3COO)2 · H2O and a solution of calciumacetate by the reaction of Ca(OH)2 withCH3COOH (glacial). The obtained solutions were mixed and stirred for 1 h at 85°C. Titanium butoxidewas added dropwise to the homogeneous solution andkept for 1 h at continuous heating (85°C) and stirring.The solution was dried in a drying cabinet at 100°Cuntil constant weight and annealed in air at temperatures200, 400, 600, 800, and 1100°C.
  • 99
  • tetrabutoxytitanium [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • zircornium(IV) n-propoxide [ No CAS ]
  • (BaZr0.2Ti0.8O3)0.55(Ba0.7Ca0.3TiO3)045 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate With acetylacetone In acetic acid Stage #2: tetrabutoxytitanium; zircornium(IV) n-propoxide In acetic acid at 100 - 200℃; Further stages; General procedure: (1-x)Ba(Zr0.20Ti0.80)O3-x(Ba0.70Ca0.30)TiO3, (x=0.45, 0.50 and 0.55) ceramics were prepared by sol-gel reaction technique. Barium acetate Ba(CH3COO)2 (>99%, Sigma Aldrich), Calcium acetate Ca(CH3COO)2 (>99%, Sigma Aldrich), Zirconium (IV) propoxide solution Zr(OCH2CH2CH3)4 (70wt% in 1-propanol, Sigma Aldrich) and Titanium (IV) butoxide (97%, Sigma Aldrich) were used as starting materials. Fig. 1 shows the flow chart of synthesis process BZT-xBCT powders by sol gel method [33]. Barium acetate and Calcium acetate were weighed according to their stoichiometry proportions and separately dissolved in acetic acid solvent followed with continuous stirring for 2h to form a transparent stable solution. Then Calcium acetate precursor solution was added dropwise into Barium acetate solution by continuous stirring, a mixed solution of Barium acetate and Calcium acetate were obtained. Afterwards, acetylacetone (99%, Sigma Aldrich) was added to this mixed solution which acts as the chelating agent. Then 0.1 molar solution of Titanium (IV) butoxide and Zirconium (IV) propoxide solution was added dropwise in the mixed solution with continuous stirring, a final solution is formed. The final solution was heated at 100°C for igniting the solvent to form a gel. After that gel is heated at 200°C to xerogel. The xerogel is calcined at 1000°C for 2h in an alumina crucible. Green pellets were prepared by adding Polyvinyl Alcohol (2wt%) binder to the calcined powder by applying 5 tons of pressure in the uniaxial hydraulic press. Finally, the green pellets were sintered at 1350°C for 4h in air. Ceramic pellets of 10mm diameter were polished up-to 0.90mm thick.
  • 100
  • tetrabutoxytitanium [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • zircornium(IV) n-propoxide [ No CAS ]
  • Ba0.85Ca0.15Zr0.1Ti0.9O3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate With acetylacetone In acetic acid Stage #2: tetrabutoxytitanium; zircornium(IV) n-propoxide In acetic acid at 100 - 200℃; Further stages; General procedure: (1-x)Ba(Zr0.20Ti0.80)O3-x(Ba0.70Ca0.30)TiO3, (x=0.45, 0.50 and 0.55) ceramics were prepared by sol-gel reaction technique. Barium acetate Ba(CH3COO)2 (>99%, Sigma Aldrich), Calcium acetate Ca(CH3COO)2 (>99%, Sigma Aldrich), Zirconium (IV) propoxide solution Zr(OCH2CH2CH3)4 (70wt% in 1-propanol, Sigma Aldrich) and Titanium (IV) butoxide (97%, Sigma Aldrich) were used as starting materials. Fig. 1 shows the flow chart of synthesis process BZT-xBCT powders by sol gel method [33]. Barium acetate and Calcium acetate were weighed according to their stoichiometry proportions and separately dissolved in acetic acid solvent followed with continuous stirring for 2h to form a transparent stable solution. Then Calcium acetate precursor solution was added dropwise into Barium acetate solution by continuous stirring, a mixed solution of Barium acetate and Calcium acetate were obtained. Afterwards, acetylacetone (99%, Sigma Aldrich) was added to this mixed solution which acts as the chelating agent. Then 0.1 molar solution of Titanium (IV) butoxide and Zirconium (IV) propoxide solution was added dropwise in the mixed solution with continuous stirring, a final solution is formed. The final solution was heated at 100°C for igniting the solvent to form a gel. After that gel is heated at 200°C to xerogel. The xerogel is calcined at 1000°C for 2h in an alumina crucible. Green pellets were prepared by adding Polyvinyl Alcohol (2wt%) binder to the calcined powder by applying 5 tons of pressure in the uniaxial hydraulic press. Finally, the green pellets were sintered at 1350°C for 4h in air. Ceramic pellets of 10mm diameter were polished up-to 0.90mm thick.
  • 101
  • tetrabutoxytitanium [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • zircornium(IV) n-propoxide [ No CAS ]
  • (BaZr0.2Ti0.8O3)0.45(Ba0.7Ca0.3TiO3)055 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: calcium acetate; barium(II) acetate With acetylacetone In acetic acid Stage #2: tetrabutoxytitanium; zircornium(IV) n-propoxide In acetic acid at 100 - 200℃; Further stages; General procedure: (1-x)Ba(Zr0.20Ti0.80)O3-x(Ba0.70Ca0.30)TiO3, (x=0.45, 0.50 and 0.55) ceramics were prepared by sol-gel reaction technique. Barium acetate Ba(CH3COO)2 (>99%, Sigma Aldrich), Calcium acetate Ca(CH3COO)2 (>99%, Sigma Aldrich), Zirconium (IV) propoxide solution Zr(OCH2CH2CH3)4 (70wt% in 1-propanol, Sigma Aldrich) and Titanium (IV) butoxide (97%, Sigma Aldrich) were used as starting materials. Fig. 1 shows the flow chart of synthesis process BZT-xBCT powders by sol gel method [33]. Barium acetate and Calcium acetate were weighed according to their stoichiometry proportions and separately dissolved in acetic acid solvent followed with continuous stirring for 2h to form a transparent stable solution. Then Calcium acetate precursor solution was added dropwise into Barium acetate solution by continuous stirring, a mixed solution of Barium acetate and Calcium acetate were obtained. Afterwards, acetylacetone (99%, Sigma Aldrich) was added to this mixed solution which acts as the chelating agent. Then 0.1 molar solution of Titanium (IV) butoxide and Zirconium (IV) propoxide solution was added dropwise in the mixed solution with continuous stirring, a final solution is formed. The final solution was heated at 100°C for igniting the solvent to form a gel. After that gel is heated at 200°C to xerogel. The xerogel is calcined at 1000°C for 2h in an alumina crucible. Green pellets were prepared by adding Polyvinyl Alcohol (2wt%) binder to the calcined powder by applying 5 tons of pressure in the uniaxial hydraulic press. Finally, the green pellets were sintered at 1350°C for 4h in air. Ceramic pellets of 10mm diameter were polished up-to 0.90mm thick.
  • 102
  • Iron(III) nitrate nonahydrate [ No CAS ]
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • [ 62-54-4 ]
  • La0.95Ca0.05FeO3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: Iron(III) nitrate nonahydrate; lanthanum(III) nitrate hexahydrate; calcium acetate With citric acid In water at 80℃; for 3 - 4h; Stage #2: at 200℃; Stage #3: at 900℃; for 10h; Calcination; General procedure: Fig. 1 depicts the specific preparation process of La1-xCaxFeO3 (x=0, 0.05, 0.1, 0.15, and 0.2) ferrite MAMs. Fe (NO3)3·9H2O, La (NO3)3·6H2O, 2(C2H3CO2) Ca, and citric acid are dissolved in deionized water and continuously stirred using a magnetic stirrer at 80°C for 3-4h for gelation reaction to form a reddish-brown gel. Next, the gel was placed in a blast drying oven at 100°C and dried for 24h to obtain a dry precursor. The dried precursor was subjected to a self-propagating reaction at 200°C using an electronic oven, and the sample was powdered using an agate mortar. Under an air atmosphere, calcined in a muffle furnace at 900°C for 10h and naturally cooled to room temperature to form ferrite MAMs.
  • 103
  • Iron(III) nitrate nonahydrate [ No CAS ]
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • [ 62-54-4 ]
  • (La0.9Ca0.1)FeO3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: Iron(III) nitrate nonahydrate; lanthanum(III) nitrate hexahydrate; calcium acetate With citric acid In water at 80℃; for 3 - 4h; Stage #2: at 200℃; Stage #3: at 900℃; for 10h; Calcination; General procedure: Fig. 1 depicts the specific preparation process of La1-xCaxFeO3 (x=0, 0.05, 0.1, 0.15, and 0.2) ferrite MAMs. Fe (NO3)3·9H2O, La (NO3)3·6H2O, 2(C2H3CO2) Ca, and citric acid are dissolved in deionized water and continuously stirred using a magnetic stirrer at 80°C for 3-4h for gelation reaction to form a reddish-brown gel. Next, the gel was placed in a blast drying oven at 100°C and dried for 24h to obtain a dry precursor. The dried precursor was subjected to a self-propagating reaction at 200°C using an electronic oven, and the sample was powdered using an agate mortar. Under an air atmosphere, calcined in a muffle furnace at 900°C for 10h and naturally cooled to room temperature to form ferrite MAMs.
  • 104
  • Iron(III) nitrate nonahydrate [ No CAS ]
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • [ 62-54-4 ]
  • La0.85Ca0.15FeO3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: Iron(III) nitrate nonahydrate; lanthanum(III) nitrate hexahydrate; calcium acetate With citric acid In water at 80℃; for 3 - 4h; Stage #2: at 200℃; Stage #3: at 900℃; for 10h; Calcination; General procedure: Fig. 1 depicts the specific preparation process of La1-xCaxFeO3 (x=0, 0.05, 0.1, 0.15, and 0.2) ferrite MAMs. Fe (NO3)3·9H2O, La (NO3)3·6H2O, 2(C2H3CO2) Ca, and citric acid are dissolved in deionized water and continuously stirred using a magnetic stirrer at 80°C for 3-4h for gelation reaction to form a reddish-brown gel. Next, the gel was placed in a blast drying oven at 100°C and dried for 24h to obtain a dry precursor. The dried precursor was subjected to a self-propagating reaction at 200°C using an electronic oven, and the sample was powdered using an agate mortar. Under an air atmosphere, calcined in a muffle furnace at 900°C for 10h and naturally cooled to room temperature to form ferrite MAMs.
  • 105
  • Iron(III) nitrate nonahydrate [ No CAS ]
  • lanthanum(III) nitrate hexahydrate [ No CAS ]
  • [ 62-54-4 ]
  • (La0.8Ca0.2)FeO3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: Iron(III) nitrate nonahydrate; lanthanum(III) nitrate hexahydrate; calcium acetate With citric acid In water at 80℃; for 3 - 4h; Stage #2: at 200℃; Stage #3: at 900℃; for 10h; Calcination; General procedure: Fig. 1 depicts the specific preparation process of La1-xCaxFeO3 (x=0, 0.05, 0.1, 0.15, and 0.2) ferrite MAMs. Fe (NO3)3·9H2O, La (NO3)3·6H2O, 2(C2H3CO2) Ca, and citric acid are dissolved in deionized water and continuously stirred using a magnetic stirrer at 80°C for 3-4h for gelation reaction to form a reddish-brown gel. Next, the gel was placed in a blast drying oven at 100°C and dried for 24h to obtain a dry precursor. The dried precursor was subjected to a self-propagating reaction at 200°C using an electronic oven, and the sample was powdered using an agate mortar. Under an air atmosphere, calcined in a muffle furnace at 900°C for 10h and naturally cooled to room temperature to form ferrite MAMs.
  • 106
  • [ 79-20-9 ]
  • [ 62-54-4 ]
YieldReaction ConditionsOperation in experiment
98.3% With water monomer; calcium(II) oxide at 45 - 60℃; for 3.5h; 1 Conversion of Methyl Acetate to Calcium Acetate To a three-necked round bottom flask placed in a heating mantle and equipped with a mechanical stirrer, temperature-measuring thermocouple, and pressure-equalizing dropping funnel, was added 15.2 g (0.26 mole) of lime (95%; Specialty Minerals, Inc), followed by enough city water (159.9 g) to make a mixable slurry. The temperature of the slurry did not exceed 45° C. To this stirred slurry was dropwise added 40.7 g (0.55 mole) of methyl acetate (96.4%; Sekisui) over a period of 1.5 hr. After this addition was complete, the reaction solution was kept at 60° for 2 hr, and then the temperature was raised to 70° C. to distill volatile components into a receiver. A total of 26.5 g of distillate was collected over a period of 2 hr. Analysis of this distillate gave 11.8 g of water by Karl Fischer titration. The volatile organic constituents of the distillate were analyzed by gas chromatography to give 11.6 g of methanol (70% recovery), and 3.1 g of unreacted methyl acetate. The remaining contents of the round bottom flask had a pH of 6.7. Upon cooling, solids were precipitated, removed by filtration, and dried in an oven to give 37.9 g of calcium acetate (98.3% yield based on 92% conversion) as a white solid. Analysis by standard Ca-EDTA titration gave a purity of 99.8%.
  • 107
  • [ 62-54-4 ]
  • 4K(1+)*4C8H18O4P(1-) [ No CAS ]
  • Ca(2+)*K(1+)*3C8H18O4P(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% In methanol at 25℃; for 24h;
  • 108
  • titanium tetra-n-butoxide [ No CAS ]
  • praseodymium(III) nitrate hexahydrate [ No CAS ]
  • [ 62-54-4 ]
  • [ 543-80-6 ]
  • barium calcium titanate [ No CAS ]
YieldReaction ConditionsOperation in experiment
With polyvinylpyrrolidone In glacial acetic acid First, an appropriate amount of glacial acetic acid and deionized water solution were added to a clean glass bottle containing magneton as the solvent. The mass ratio of glacial acetic acid to deionized water was 3:1. Then, a certain amount of barium acetate particles were weighed and placed in a glass bottle filled with solvent. The glass bottle was put into a magnetic mixer for full stirring. When all barium acetate particles were dissolved, calcium acetate particles were added to the solvent for dissolution. The chemical dose ratio of barium acetate and calcium acetate was 7:3. After the calcium acetate granules were completely dissolved, praseodymium nitrate granules were added to the solvent. The doping ratio of praseodymium nitrate was 0.2%. Subsequently, 5wt% PVP was added to the solvent for dissolution. Finally, the corresponding stoichiometric solution of tetrabutyl titanate was added to the glass bottle, and then the solution in the bottle was fully fused until a stable sol was formed, at which point electrostatic spinning begins.
  • 109
  • iron(III) nitrate monohydrate [ No CAS ]
  • [ 62-54-4 ]
  • calcium ferrite [ No CAS ]
YieldReaction ConditionsOperation in experiment
With polyethylene glycol In lithium hydroxide monohydrate at 120 - 1050℃; for 12h; 1.2 (2) CaFe2O4 synthesis using a solution-based method In a typical process for synthesizing calcium ferrite (CaFe2O4, CFO) particles,2 mmol of calcium acetate monohydrate and 4 mmol of iron (III) nitrate monohydrate were dissolved in 20 mL of water,5 mL of an aqueous solution of polyethylene glycol (5% by weight) was added into the obtained solution.The final solution was vigorously stirred at 120° C. for 2 hours.The dried powders were then calcined at 450° C. for 2 hours and at 1,050° C. for an additional 10 hours.The CFO film was prepared by a typical doctor-blade method,A dense CFO paste was prepared using 1.0 g of the synthesized CFO powder mixed with a solution of 0.5 g of polyethylene glycol (PEG 8000) in 1.5 mL of distilled water.The obtained mixture was subjected to intense-sonic treatment for 10 minutes, and then the prepared CFO paste was coated on Ti foil using a doctor blade method.Thereafter, the prepared film was calcined at various temperatures in an Ar atmosphere (flow rate 20 sccm).
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