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CAS No. : | 1113-38-8 | MDL No. : | MFCD00013308 |
Formula : | C2H8N2O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | VBIXEXWLHSRNKB-UHFFFAOYSA-N |
M.W : | 124.10 | Pubchem ID : | 14213 |
Synonyms : |
|
Num. heavy atoms : | 8 |
Num. arom. heavy atoms : | 0 |
Fraction Csp3 : | 0.0 |
Num. rotatable bonds : | 1 |
Num. H-bond acceptors : | 4.0 |
Num. H-bond donors : | 2.0 |
Molar Refractivity : | 23.36 |
TPSA : | 80.26 Ų |
GI absorption : | Low |
BBB permeant : | No |
P-gp substrate : | Yes |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -11.51 cm/s |
Log Po/w (iLOGP) : | 0.0 |
Log Po/w (XLOGP3) : | -6.27 |
Log Po/w (WLOGP) : | -2.76 |
Log Po/w (MLOGP) : | -10.52 |
Log Po/w (SILICOS-IT) : | -0.97 |
Consensus Log Po/w : | -4.11 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 3.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | 3.41 |
Solubility : | 317000.0 mg/ml ; 2550.0 mol/l |
Class : | Highly soluble |
Log S (Ali) : | 5.27 |
Solubility : | 23100000.0 mg/ml ; 186000.0 mol/l |
Class : | Highly soluble |
Log S (SILICOS-IT) : | 1.47 |
Solubility : | 3660.0 mg/ml ; 29.5 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 1.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 1.21 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; at 45℃; for 8h; | K2[PtCl4] (59.60g) is dissolved in water (439 ml). Potassium iodide (168.0 g) is dissolved in water (147 ml). Both solutions are purified and stirred for 30 min. Trans-I-1,2-diaminocyclohexane (18.39 g) is dissolved in water (72 ml.) The solution is added to the platinum-containing solution while stirring and the agitation is continued for 72 hours. The obtained suspension is filtered. The filtered deposit is washed with water six times (200 ml) and subsequently dried. Yield of 1,2-diamonocyclohexane-diiodoplatinum II: 77.9 g (96%). The obtained Trans-1-1,2 diaminocyclohexane-diiodo-platinum(II) is suspended in water (1389 ml) and the suspension is heated at 45 degrees C. Silver nitrate (43.91 g) is dissolved in water (139 ml) and this solution is purified with platinum-containing solution. The resulting mixture is agitated for 8 hours at 45 degrees C. The suspension is subsequently cooled within 6 hours at 6 degrees C. and filtered. Di-<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (20.19 g) is dissolved in water (278 mL). Water (3333 mL), <strong>[1113-38-8]ammonium oxalate</strong> solution and platinum-containing solution are purified and agitated for 8 hours at 45 degrees C. Subsequently activated carbon is added (3.05 g) and again further agitated for 16 hours. It is filtered and the active carbon treatment is repeated. The obtained solution is then led through a sterile filter into a rotary evaporator and concentrated at 55 to 65 degrees C. in a vacuum to about 110 ml. The obtained suspension is filtered and the deposit is agitated thrice in water (28 ml) for 10 min. Subsequently it is washed thrice with methanol (139 ml). The filtered deposit is dried in sterile air stream for at least 24 hours. Yield of oxalato (trans-1-1,2-diaminocyclohexane) platinum (II): 33.88 g (80%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With silver sulfate; In acetonitrile; for 14h;Schlenk technique; Darkness; | A mixture of trans-[PdCl2(L)2] (0.10 g, 0.17 mM), Ag2SO4 (0.054 g, 0.17 mM), and (NH4)2C2O4 (0.030 g, 0.24 mM) in dry CH3CN (50 mL) was stirred for 14 h in the dark. The solution was centrifuged and filtered through Celite. The solvent was evaporated andthe resulting residue was extracted with 5 mL of CH2Cl2. The yellow solid was precipitatedwith hexane, filtered, washed with diethyl ether (5 mL), and dried in vacuum. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With cetyltrimethylammonim bromide; butan-1-ol; In 2,2,4-trimethylpentane; for 15h; | ThO2 nanoparticles were synthesized by the thermal decomposition of thorium oxalate precursor using the method reported in our earlier work for synthesis of nickel oxalate [22]. The precursors were synthesized by the reverse micellar route with CTAB (cetyl trimethyl ammonium bromide) as the surfactant, 1-butanol as the co-surfactant and iso-octane as the nonpolar solvent. The weight fraction of various constituents in the microemulsion was 16.76% of CTAB, 13.9% of n-butanol, 59.29% of isooctane, and 10.05% of aqueous phase. For the synthesis of thorium oxalate precursor two different microemulsion, one containing 0.1M aqueous solution of thorium nitrate and the other containing the aqueous solution of <strong>[1113-38-8]ammonium oxalate</strong> were slowly mixed and stirred for 15h. The product was separated from microemulsion by centrifugation and washed with 1:1 mixture of chloroform and methanol and dried at room temperature. The product was decomposed at 500C for 6h to obtain thorium oxide. For preparation of samarium doped sample, appropriate quantities (1mol%) of samarium nitrate, Sm (NO3)3 were added at the initial stage in thorium nitrate microemulsion. Thorium nitrate (99.99%) and 1mol% of samarium nitrate (99.99%) were dissolved in quartz double distilled and stirred for 2h at 80-90. Based on ionic radii analogy composition is like Th1-xSmxO2, samarium occupies thorium site. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
34.65% | In N,N-dimethyl-formamide; for 22h;Inert atmosphere; Glovebox; | Synthesis of [(CpPOEtCo)V(OH)]2(mu-ox), (ox = oxalato), 4 An amount of 0.502 g of 3, (CpPOEtCo)VCl2(DMF) (0.688 mmol) was dissolved in 10 mL of N,N-dimethylformamide. The same amount of DMF was added to a flask containing 0.099 g of <strong>[1113-38-8]ammonium oxalate</strong> (0.695 mmol). The oxalate slurry was added to the solution of (CpPOEtCo)VCl2(DMF) resulting in a solution that gradually turned yellow-green, which was stirred for 22 h. The solvent was removed in vacuo, resulting in a green residue that was extracted into 20 mL of diethyl ether and gravity filtered. The solvent was allowed to evaporate yielding bright green crystals suitable for X-ray diffraction. Yield: 0.154 g (0.119 mmol, 34.65%). MP, dec. 212 C. Anal. Calc. for C36H72Co2O24P6V2 (1294.5344): C, 33.5; H, 5.5. Found: C, 33.9; H, 5.7%. IR (cm-1): 2980, 2930, 1680, 1388, 1262, 1128, 1031, 1069, 976, 930, 906, 835, 808, 771, 728. Mag. Suscept. mueff (muB): 2.17; chim = 0.0020 erg G-2 mol-1 (chimT = 0.59). Single crystals of this compound were additionally analyzed using X-ray diffraction. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
38% | In N,N-dimethyl-formamide; for 12h;Inert atmosphere; Glovebox; | Synthesis of [(CpPOEtCo)VCl]2(mu-ox), 5 (ox = oxalato) An amount of 0.404 g of (CpPOEtCo)VCl2(DMF) [3] , (0.553 mmol) was dissolved in 15 mL of DMF. The same amount of DMF was added to a flask containing 0.079 g of <strong>[1113-38-8]ammonium oxalate</strong> (0.554 mmol). The solution of (CpPOEtCo)VCl2(DMF) was added to the oxalate slurry, resulting in a solution that gradually turned yellow-green. The reaction was stirred under nitrogen for 12 h, then filtered via canula. The resulting green residue was extracted with 20 mL of dichloromethane, filtered, and reduced to dryness in vacuo. The final green residue was triturated with three 15 mL portions of dry ether, Yield: 0.277 g (0.208 mmol, 38%). mp, dec. >168 C. Anal. Calc. for C36H70Co2O22P6V2 (1292.52): C, 32.47; H, 5.30. Found: C, 33.65; H, 5.33%. IR (cm-1): 2980, 2930, 2906, 1708, 1650, 1476, 1441, 1425, 1387, 1364, 1349, 1261, 1160, 1103, 1075, 1010, 971, 922, 836, 796, 769, 729. Magnetic Susceptibility mueff (muB): 3.17; chim = 0.00415 erg G-2 mol-1 (chimT = 1.22). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ammonium hydroxide; In water; at 60℃; for 18h;pH 8;Green chemistry; | In a typical synthesis, MnCl2*4H2O (2.97 g), (NH4)2C2O4 (1.95 g) and PVP (0.15 g) was dissolved in water(70 mL) and then heated to 60 C. After a few minutes, ammonia solution was dropped slowly into the mixture to adjust thepH value to 8.0. The obtained solution was then incubated for 18 hat 60 C. The precipitate obtained after the incubation process was filtered and washed multiple times with water and butanol. Finallythe product was dried at 90 C for 12 h. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
MnSO4.H2O and (NH4)2C2O4.H2O with a mole ratio of 1:1.2 were mixed and well ground in a mortar atroom temperature. In the grinding process, the solid-state reaction took place, accompanying with thecrystalline water releasing gradually from the starting materials. Ground for 40 min, the wet mixture wastransferred to a thermostatic water bath of 80 oC for several hours, and then a dry mixture was obtained.The mixture was washed with distilled water to remove the dissoluble substances, and dried in an oven at110 oC for 10 h, and then a white MnC2O4 precursor was obtained. The precursor was calcined in atmosphereat 400 oC in a muffle furnace at 10 h for oxidative decomposition. Afterwards, the calcined product(manganese oxide) was subjected to acid-treatment in 2M H2SO4 solution at 80 oC for 2h under magneticstirring, in order to increase its degree of oxidation. After that, the product was washed thoroughly withdistilled water, filtered, dried at 105 oC, and then a final product (MnO2 material) was obtained. | ||
at 20℃; for 0.666667h;Milling; | Briefly, a mixture of MnSO4*H2O (1 mmol, 0.169 g) and (NH4)2C2O4*H2O (1.2 mmol, 0.17 g) was mixed and ground in a mortar at room temperature for 40 min. For drying the wet mixture, it was placed in a water bath of 80 oC for several hours. The obtained dry mixture was washed with distilled water to remove the unreacted substances and dried at 110 oC for 10 h. Then, the resulted white solid was calcined to produce manganese oxide in atmosphere at 400 C for 10 h. Afterwards, the resulted MnO2 was added to a 2 M H2SO4 solution and stirred at 80 oC for 2 h in order to increase its degree of oxidation. The product was filtered and washed with distilled water and finally dried at 105 oC to obtain the target MnO2 nanoparticles. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In2O3 can be prepared using <strong>[1113-38-8]ammonium oxalate</strong> in place of oxalic acid. 16.90 g In(NO3)3.5 H2O was dissolved in 50 mL H2O. 9.21 g <strong>[1113-38-8]ammonium oxalate</strong> was dissolved in 85 mL H2O with gentle heating. Addition of the <strong>[1113-38-8]ammonium oxalate</strong> to the indium nitrate solution resulted in the formation of a thick white precipitate. The volume of the mixture was reduced by gentle evaporation and the remaining slurry was placed into an oven at 90 C. to dry overnight. The resulting solid was then heated to 550 C. at 2 C./min, held for 6 h, then cooled to 25 C. at about 3 C./min. The fluffy yellow solid was pelletized and sieved to a 60-100 mesh fraction for catalyst testing (Table 37 in Example 5) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
< 30% | at 180℃; for 48h;Autoclave; | Neodymium nitrate hexahydrate (0.44g, 1.0mmol), (NH4)2C2O4·H2O (0.07g, 0.5mmol) and succinic acid (0.12g, 1.0mmol) were added to a 120mL Teflon container with 10.0mL of DI water. The Teflon container was then sealed in a stainless steel pressure Par vessel and left in a 180C oven for 48h. Two types of light pink crystalline products were obtained after slow cooling (C/h) to room temperature. Complex 2 was crystallized as fine needles with estimated yield of less than 30%. Complex 3 was crystallized as poor quality large crystals with approximately 35% yield. Recrystallization of 3 in aqueous solution was attempted. However, no obvious improvement of crystal quality could be achieved. (0016) As 2 and 3 were formed in the same reaction mixture, small amounts of 3 were manually separated for further characterizations whilst the fine needle of complex 2 was only characterized by single crystal X-ray diffraction. The powder X-ray diffraction (PXRD) patterns of 1 and 3 (Fig. S1) obtained from the bulk materials match the patterns generated from the single crystal data, suggesting that 1 and 3 in pure phase form have been obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; for 24h;Inert atmosphere; | 0.1 mol (29.08 g) of Ni(NO3)2*6H2O, 0.1 mol (29.70 g) of Co(NO3)2*6H2O, and 0.1 mol (24.76 g) of Mn(CH3COO)2*4H2O were dissolved in 150 mL H2O, and stirred at 200 rpm. 0.3 mol (43.06 g) of (NH4)2C2O4*H2O were added to the precursor mixture solution with argon atmosphere for 24 h. The obtained Ni1/3Co1/3Mn1/3C2O4*xH2O were washed by using methanol (CH3OH) and chloroform (CHCl3) and dried at 100 C for 2 h for TGA. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With barium(II) chloride dihydrate; at 20℃; | The compoundwasobtainedbydropwiseadditionof500mLof a0.2MsolutionofBaCl2 · 2H2O to500mLofa0.2Msolution at(NH4)2C2O4 ·H2O, understirringandatroomtemperature. Thewhitecrystallinepowderwasfilteredoff,washed withwater,anddriedinairatroomtemperature. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 12℃; for 504h;pH 1; | Crystals of I were obtained by slow evaporation. The compound was synthesized from a mixture of potassium nitrate, iron nitrate, and di<strong>[1113-38-8]ammonium oxalate</strong> respectively (3:1:3 molar ratio), dissolved in deionized water. This solution was acidified by arsenic acid until the pH = 1. After three weeks, the evaporation of the final mixture at a temperature of 12C led to the formation of parallelepiped green crystals identified at the title compound. A single crystal obtained in this way was chosen for X-ray diffraction studies. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
44% | 2, 5-di(2?,4?-dicarboxylphenyl) pyridine (0.041 g, 0.1 mmol) and(NH4)2C2O4·H2O (0.016 g, 0.1 mmol) in a solution of water/DMF (v/v = 4.0,12 mL) were mixed with an aqueous solution (10 mL) of Mn(CH3COO)2·4H2O (0.0295 g, 0.12 mmol). After stirring for 20 min in air, the pH value was adjusted to5.5 with nitric acid, and the mixture was placed into 25 mL Teflon-lined autoclaveunder autogenous pressure being heated at 145 C for 72 h, then the autoclavewas cooled over a period of 24 h at a rate 5 C/h. After filtration, the product waswashed with distilled water and then dried, colorless crystals of title polymerwere obtained suitable for X-ray diffraction analysis. Yield: 0.011 g (44% based onMn element)). Elemental analysis (%): calcd for C44H36Mn4N2O28: C 41.93, H 2.88,N 2.22, O 35.54, Mn 17.43, found: C 40.86, H 2.49, N 2.14, O 35.39, Mn 17.36. IR(KBr pellet, cm-1): 3486 (br), 1708(s), 1643(s), 1603(s), 1410(m), 1387(s),1139(m), 817(s), 784(m), 668(s), IR spectra see Fig. S1 for details. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
prepared with distilled water at a concentration of iron (II) 28g / 500ml L of ferrous sulfate solution was added × 10 5-3mol ascorbic solid, after stirring for 2 hours;(2) with distilled water oxalate ion concentration of 44g / 500ml L of <strong>[1113-38-8]ammonium oxalate</strong> solution;(3) controlling said <strong>[1113-38-8]ammonium oxalate</strong> solution 50 , the stirring in step (1) obtained was added thereto and stirred for 1 hour, a yellow mixed solution was filtered, the precipitate was washed with distilled water 3 to 4 times, and dried at 110 give ferrous oxalate product.After testing (the same way as in Example 1) the sample, ferrous oxalate purity of 99.7%, ferrous oxalate crystal form of a single orthorhombic structure, ferrous oxalate particle shape is a square column. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ammonium hydroxide; at 70℃; for 3h;pH 5; | To synthesize the (Fe1/3Mn2/3)C2O4 ·H2O precursor, stoichiometric amounts of FeSO4 · 7H2O, and MnSO4 ·H2O were dissolved in distilled water to a concentration of 0.5 mol dm-3. This metal solution was then dropped into a continuously stirring solution of <strong>[1113-38-8]ammonium oxalate</strong>. At the same time, an appropriate amount of NH4OH solution was added into the beaker to adjust the pH value to 5. The concentration of the solution, pH, temperature, and stirring speed were carefully controlled. The co-precipitation solution was continuously stirred for 3 h while keeping the temperature constant at 70C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ascorbic acid; In water; at 60℃; for 5h;pH 5;Inert atmosphere; | weight 180.91g ferrous acetate, 363.22g manganese tetrahydrate acetate, ascorbic acid 1.5g, dissolved in appropriate amount of water that is preparation of iron and manganese mixed solution A; 14.63g copper nitrate, dissolved in small amount of water, this is solution B. Into the reaction flask added the 402 g of <strong>[1113-38-8]ammonium oxalate</strong> and appropriate amount of water, Ammonium oxalate concentration is 1.0mol / L, into the reaction flask pass nitrogen, flow meter set at 600 ml / min, system pH is 5, the reactor temperature is controlled at 60 C and heated to <strong>[1113-38-8]ammonium oxalate</strong> completely dissolved. In the agitation state, simultaneous added the iron and manganese mixed solution A and copper nitrate solution B to the system by using parallel flow method. The drip rate of iron-manganese mixed solution A is 4 L / h, and the drip rate of copper sulfate solution B is 0.5L / h, 1L / h, 2L / h gradually increased, after the drop, in the state of stirring to continue aging 5h, stirring speed is 100r / min, the intermediate is washed with methanol, respectively, dry at 75 C, where dry time will be 3 hours, the chemical composition is Fe0.4Mn.57Cu0.03C2O4 . 2H2OCopper gradient doped intermediates, that is D50 is 100muM, see SEM fig1 in D. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen; In water; at 75℃; for 4h;pH 5; | weight 233.87g ferrous nitrate hexahydrate, 209.36 manganese tetrahydrate nitrate, dissolved in appropriate amount of water that is preparation of iron and manganese mixed solution A; weight 18.20g Nickel sulfate heptahydrate, 13.95g Magnesium acetate tetrahydrate, dissolved in water, this is solution B. Into the reaction flask added the 426 g of <strong>[1113-38-8]ammonium oxalate</strong> and appropriate amount of water, Ammonium oxalate concentration is 1.4mol / L, into the reaction flask pass hydrogen, flow meter set at 600 ml / min, system pH is 5, the reactor temperature is controlled at 75 C and heated to <strong>[1113-38-8]ammonium oxalate</strong> completely dissolved. In the agitation state, simultaneous added solution A and solution B to the system by using parallel flow method. The drip rate of iron-manganese mixed solution A is 4 L / h, and the drip rate of nickel and magnesium mixed solution B is 0.5L / h, 0.5L / h, 1L / h gradually increased, after the drop, in the state of stirring to continue aging 4h, stirring speed is 500r / min, the intermediate is washed with water, respectively, dry at 100 C, where dry time will be 6 hours, the chemical composition is 2H20 Nickel - magnesium composite gradient - doped ferric oxalate intermediate, that is D50 is 80muM, see SEM fig1 in E |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; for 3h;pH 6;Inert atmosphere; Heating; | Weighed 144.59g ferrous sulfate heptahydrate,351.52g of hydrated manganese sulphate,Soluble in the amount of water,Preparation of iron and manganese mixed solution A.To the kettle was added 402 g of <strong>[1113-38-8]ammonium oxalate</strong> and water,Ammonium oxalate concentration of 1.0mol / L,The reaction vessel was passed with nitrogen,Flowmeter set to 600ml / min,System pH 6,The reactor temperature is controlled at 65 C,Heated to <strong>[1113-38-8]ammonium oxalate</strong> completely dissolved.And then to the system by the parallel drop of iron and manganese mixed solution A,Solution A was added at a rate of 1 L / h,After dripping,Stirring in the state of aging 3h,Stirring speed of 1500r / min.The intermediate was washed with water and ethanol, respectively,85 C dry,Drying time is 5 hours,Chemical composition of Fe0.2Mn0.8C2O4 · 2H2O. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen; In ethanol; water; acetylacetone; at 65℃; for 5h;pH 6; | Weigh 117g ferrous oxalate dihydrate,Acid dihydrate 337.84g oxalyl manganous,Soluble in the amount of water,Preparation of iron and manganese oxalate dihydrate mixed solution A;Weigh 17.69 g of tetrabutyl titanate,9.69g anhydrous ethanol,1.04 g of acetylacetone,Add appropriate amount of water,Magnetic stirring,Made of titanium sol.To the kettle was added 402 g of <strong>[1113-38-8]ammonium oxalate</strong> and water,Ammonium oxalate concentration of 1.1mol / L,To the reactor into the hydrogen,Flowmeter set to 600ml / min,System pH 6,The reactor temperature is controlled at 65 C,Heated to <strong>[1113-38-8]ammonium oxalate</strong> completely dissolved.In the agitation state,Adding the iron-manganese mixed solution A and the titanium sol B to the system by the method of adding the co-Iron and manganese mixed solution A drip rate of 2L / h,While the slow drop of titanium sol B,Drip by 0.005L / h,0.025L / h, 0.05L / h gradually increased,Dripping in the state of stirring to continue aging 5h,Stirring speed of 1000r / min,The intermediate was washed with water and methanol, respectively Polyester,70 dry,Drying time is 4 hours,chemical composition of Fe0.25Mn0.73Ti0.02C2O4 · 2H2O titanium gradient doped iron oxalate was prepared |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
To prepare the anionic part (Fig. 2), an ethanolic solution (15 ml) of 1,10-phenanthroline (1 mmol, 0.198 g) was added to NiCl2*2H2O (1 mmol, 0.129 g) dissolved in distilled water (15 ml) and simultaneously an aqueous solution of <strong>[1113-38-8]ammonium oxalate</strong> (3 mmol, 0.426 g) was added to a solution of CrCl3*2H2O (2 mmol, 0.520 g) dissolved in distilled water. Both solutions were refluxed separately for 12 h and then they were mixed. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66.96% | In methanol; at 20℃; for 3h; | This compound was first obtained as an unexpected product from the following procedure: To a stirring solution of toltrz (150?mg, 0.8?mmol) in methanol (3?mL) was added an 5?mL aqueous solution of Fe(ClO4)2·6H2O (80?mg, ?0.3?mmol). The solution turned from colorless to a slightly dark reddish solution. Then a two spatula-amount (?70?mg) of ascorbic acid was added to prevent possible oxidation process. The reaction mixture was stirred at 60?C for 3?h before filtrated with rapid filter paper. The obtained clear reddish solution was kept in a small vial and left stand still to evaporate the solvent slowly. After three weeks, light yellow needle-like crystals of 1 were deposited at the bottom of the vial. After removing the mother liquid, the single crystals were quickly dried in an argon stream, and stored under argon. Yield: 35.7?mg (34.80% based on Fe). The oxalate anion seen from the X-ray diffraction result violates the basic starting materials that we put into the reaction in the first place. The only explanation is that it came from the decomposition of the ascorbic acid when it was working against the oxidation of FeII ions. There are several reports regarding this way to achieve the oxalate as coordinating ligand [14] We thus tried to prepare the oxalate compound by using (NH4)2(C2O4) (38?mg, ?0.3?mmol, with the ratio of 1:1 compared to Fe) on purpose instead of ascorbic acid in a rather mild reaction conditions (stirred at r.t.). Same light-yellow crystals formed after one week with a higher yield of 66.96% (68.7?mg, based on Fe). Anal. Calc. (Found) for C22H30FeN8O11: C, 41.39 (41.44); H, 4.74 (4.59); N, 17.55 (17.57). IR (KBr) n/cm-1: 3115 (m), 2921 (w), 1643 (vs), 1605 (s), 1523 (m), 1421 (w), 1122 (m), 829 (m), 619 (m), 489 (w). C22H30FeN8O9. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72.98% | In methanol; at 20℃; for 3h; | This compound was first obtained as an unexpected product from the following procedure: To a stirring solution of toltrz (150?mg, 0.8?mmol) in methanol (3?mL) was added an 5?mL aqueous solution of Fe(ClO4)2·6H2O (80?mg, ?0.3?mmol). The solution turned from colorless to a slightly dark reddish solution. Then a two spatula-amount (?70?mg) of ascorbic acid was added to prevent possible oxidation process. The reaction mixture was stirred at 60?C for 3?h before filtrated with rapid filter paper. The obtained clear reddish solution was kept in a small vial and left stand still to evaporate the solvent slowly. After three weeks, light yellow needle-like crystals of 1 were deposited at the bottom of the vial. After removing the mother liquid, the single crystals were quickly dried in an argon stream, and stored under argon. Yield: 35.7?mg (34.80% based on Fe). The oxalate anion seen from the X-ray diffraction result violates the basic starting materials that we put into the reaction in the first place. The only explanation is that it came from the decomposition of the ascorbic acid when it was working against the oxidation of FeII ions. There are several reports regarding this way to achieve the oxalate as coordinating ligand [14] We thus tried to prepare the oxalate compound by using (NH4)2(C2O4) (38?mg, ?0.3?mmol, with the ratio of 1:1 compared to Fe) on purpose instead of ascorbic acid in a rather mild reaction conditions (stirred at r.t.). Same light-yellow crystals formed after one week with a higher yield of 66.96% (68.7?mg, based on Fe). Anal. Calc. (Found) for C22H30FeN8O11: C, 41.39 (41.44); H, 4.74 (4.59); N, 17.55 (17.57). IR (KBr) n/cm-1: 3115 (m), 2921 (w), 1643 (vs), 1605 (s), 1523 (m), 1421 (w), 1122 (m), 829 (m), 619 (m), 489 (w). C22H30FeN8O9. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | With sodium hydroxide; In ethanol; at 140℃; for 72h;Autoclave; High pressure; | General procedure: Complexes 5-8 were prepared by a similar procedure as those for 1-4. A solution of H3pdc (0.032g, 0.2mmol), (NH4)2C2O4·H2O (0.015g, 0.1mmol) and NaOH (0.004g, 0.1mmol) in H2O/ EtOH (v/v=1.5, 10mL) were mixed with an aqueous solution (10mL) of lanthanide salt (Ce(NO3)3·6H2O for 5, PrCl3·6H2O for 6, NdCl3·6H2O for 7, Sm(NO3)3·6H2O for 8, 0.2mmol). After stirring for 20min, the mixture was placed into 25mL Teflon-lined autoclave under autogenous pressure and heated at 140C for 3days, then cooled to the ambient temperature at the rate of 5Ch-1. After filtration, the products were washed with distilled water and then dried, finally the target products (colorless for 5, green for 6, peach for 7 and yellow for 8) were obtained. 5: Yield 0.043g (54%, based on the Ce(III)). Elemental analysis calcd (%) for C6H8CeN2O9: C, 18.40; H, 1.79; N, 7.16. Found: C, 18.31; H, 1.88; N, 7.10. IR (KBr, disk): 3586(s), 3357(vs), 3124(s), 2916(s), 1670(s), 1577(vs), 1426(vs), 1349(vs), 1121(s), 1110(s), 957(m), 857(s), 815(s), 737(s)cm-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | With sodium hydroxide; In ethanol; at 140℃; for 72h;Autoclave; High pressure; | General procedure: Complexes 5-8 were prepared by a similar procedure as those for 1-4. A solution of H3pdc (0.032g, 0.2mmol), (NH4)2C2O4·H2O (0.015g, 0.1mmol) and NaOH (0.004g, 0.1mmol) in H2O/ EtOH (v/v=1.5, 10mL) were mixed with an aqueous solution (10mL) of lanthanide salt (Ce(NO3)3·6H2O for 5, PrCl3·6H2O for 6, NdCl3·6H2O for 7, Sm(NO3)3·6H2O for 8, 0.2mmol). After stirring for 20min, the mixture was placed into 25mL Teflon-lined autoclave under autogenous pressure and heated at 140C for 3days, then cooled to the ambient temperature at the rate of 5Ch-1. After filtration, the products were washed with distilled water and then dried, finally the target products (colorless for 5, green for 6, peach for 7 and yellow for 8) were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With sodium hydroxide; In ethanol; at 140℃; for 72h;Autoclave; High pressure; | General procedure: Complexes 5-8 were prepared by a similar procedure as those for 1-4. A solution of H3pdc (0.032g, 0.2mmol), (NH4)2C2O4·H2O (0.015g, 0.1mmol) and NaOH (0.004g, 0.1mmol) in H2O/ EtOH (v/v=1.5, 10mL) were mixed with an aqueous solution (10mL) of lanthanide salt (Ce(NO3)3·6H2O for 5, PrCl3·6H2O for 6, NdCl3·6H2O for 7, Sm(NO3)3·6H2O for 8, 0.2mmol). After stirring for 20min, the mixture was placed into 25mL Teflon-lined autoclave under autogenous pressure and heated at 140C for 3days, then cooled to the ambient temperature at the rate of 5Ch-1. After filtration, the products were washed with distilled water and then dried, finally the target products (colorless for 5, green for 6, peach for 7 and yellow for 8) were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | With sodium hydroxide; In ethanol; at 140℃; for 72h;Autoclave; High pressure; | General procedure: Complexes 5-8 were prepared by a similar procedure as those for 1-4. A solution of H3pdc (0.032g, 0.2mmol), (NH4)2C2O4·H2O (0.015g, 0.1mmol) and NaOH (0.004g, 0.1mmol) in H2O/ EtOH (v/v=1.5, 10mL) were mixed with an aqueous solution (10mL) of lanthanide salt (Ce(NO3)3·6H2O for 5, PrCl3·6H2O for 6, NdCl3·6H2O for 7, Sm(NO3)3·6H2O for 8, 0.2mmol). After stirring for 20min, the mixture was placed into 25mL Teflon-lined autoclave under autogenous pressure and heated at 140C for 3days, then cooled to the ambient temperature at the rate of 5Ch-1. After filtration, the products were washed with distilled water and then dried, finally the target products (colorless for 5, green for 6, peach for 7 and yellow for 8) were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; at 20 - 80℃; for 8h; | Weigh 100.0g (0.478mol) of dichlorodiammine palladium into a 2000mL beaker.Add 1200 mL of deionized water and stir.And adding ammonia water to completely dissolve to obtain 1400 g of dichlorotetraammine palladium solution.While stirring the dichlorotetraammine palladium (II) solution,Slowly add 200g (1.612mol) of <strong>[1113-38-8]ammonium oxalate</strong>,A white precipitate appeared,Continue to stir the reaction for 4h,Allow to stand for 10 min filtration,A white solid was obtained.Add this white solid to 1300 mL of deionized water.Heat to 80 C until the solids are completely dissolved,When cooled to room temperature,Add 200.0 g (1.612 mol) of <strong>[1113-38-8]ammonium oxalate</strong>,Stir for 4h,Allow to stand for 30 min filtration,Washed twice with a small amount of deionized water.Obtaining pure white oxalic acid tetraammine palladium solid,This process can effectively remove chloride ions in the solution.And no other impurity ions are introduced;Slowly add 35% acetic acid 500 mL to the pure white oxalic acid tetraammine palladium solid.The reaction is heated to 50-60 C for 0.5 h without bubbles.The insoluble matter is removed by filtration to obtain a pure tetraammine palladium acetate solution.Concentrated under reduced pressure to50mL of concentrate,The concentrate was added to 1000 mL of organic alcohol to crystallize under stirring.Obtained a pale yellow transparent crystal,After filtration, it was washed with 200 mL of organic alcohol and dried under vacuum at 80 C for 2 h.Obtained 131.56 g of tetraammine palladium acetate.The yield was 95.67%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
The catalysts was synthesized by an oxalate route following the latest research described in the literature [1,2]. In the typical synthesis, using water was high purity water (16 MOmegacm-1). Ammonium oxalate solution (100 mL 0.24 M) was quickly added to manganous nitrate solution (100 mL 0.2 M) under strong stirring at room temperature. After the mixture was stirred for 40 min, the white precipitate (Precursor) was obtained by filtration. Subsequently, the precipitate was washed several times with high purity water (16 MOmegacm-1) and absolute ethanol. Then, the precipitate was dried at 80 C for 20 h. The obtained product was calcined at a certain temperature (350 C, 450 C, 550 C) for 5 h under air atmosphere with a heating ramp of 2 C*min-1. The calcined sample were denoted M-3, M-4, M-5. |
Tags: 1113-38-8 synthesis path| 1113-38-8 SDS| 1113-38-8 COA| 1113-38-8 purity| 1113-38-8 application| 1113-38-8 NMR| 1113-38-8 COA| 1113-38-8 structure
[ 867-56-1 ]
Sodium (S)-2-hydroxypropanoate
Similarity: 0.52
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