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[ CAS No. 24605-36-5 ] {[proInfo.proName]}

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Chemical Structure| 24605-36-5
Chemical Structure| 24605-36-5
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Product Details of [ 24605-36-5 ]

CAS No. :24605-36-5 MDL No. :MFCD00078393
Formula : C6H6NNaO6S2 Boiling Point : -
Linear Structure Formula :- InChI Key :SYFQTIIOWUIZGU-UHFFFAOYSA-M
M.W : 275.23 Pubchem ID :44118805
Synonyms :

Calculated chemistry of [ 24605-36-5 ]

Physicochemical Properties

Num. heavy atoms : 16
Num. arom. heavy atoms : 6
Fraction Csp3 : 0.0
Num. rotatable bonds : 2
Num. H-bond acceptors : 6.0
Num. H-bond donors : 2.0
Molar Refractivity : 48.71
TPSA : 154.35 Ų

Pharmacokinetics

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) : -11.69 cm/s

Lipophilicity

Log Po/w (iLOGP) : -3.9
Log Po/w (XLOGP3) : -5.22
Log Po/w (WLOGP) : 1.59
Log Po/w (MLOGP) : -0.2
Log Po/w (SILICOS-IT) : -1.96
Consensus Log Po/w : -1.94

Druglikeness

Lipinski : 0.0
Ghose : None
Veber : 1.0
Egan : 1.0
Muegge : 2.0
Bioavailability Score : 0.11

Water Solubility

Log S (ESOL) : 1.6
Solubility : 10900.0 mg/ml ; 39.5 mol/l
Class : Highly soluble
Log S (Ali) : 2.62
Solubility : 116000.0 mg/ml ; 421.0 mol/l
Class : Highly soluble
Log S (SILICOS-IT) : -0.74
Solubility : 49.6 mg/ml ; 0.18 mol/l
Class : Soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 2.0 alert
Leadlikeness : 0.0
Synthetic accessibility : 2.68

Safety of [ 24605-36-5 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P264-P280-P302+P352+P332+P313+P362+P364-P305+P351+P338+P337+P313 UN#:N/A
Hazard Statements:H315-H319 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 24605-36-5 ]

* 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 [ 24605-36-5 ]

[ 24605-36-5 ] Synthesis Path-Downstream   1~48

  • 1
  • [ 108-77-0 ]
  • [ 24605-36-5 ]
  • [ 107-15-3 ]
  • [ 742062-32-4 ]
YieldReaction ConditionsOperation in experiment
59.3% (1) Synthesis of the compound of the following formula (13) (a compound of the formula (4) where X is a 2,5-disulfoanilino group, Y is an amino group and E is ethylene); [Show Image] In 2000 parts of ice water, 7.2 parts of LOTAT OH104-K (which is a trade name, manufactured by Lion Corporation) and 239.9 parts of cyanuric chloride were added and stirred for 30 minutes. Next, 411.6 parts of <strong>[24605-36-5]aniline-2,5-disulfonic acid monosodium salt</strong> (purity: 91.2%) is added thereto, and reaction was carried out at 10 to 15C for 1 hour and at 27 to 30C for 2 hours while adding a 25% sodium hydroxide aqueous solution to maintain pH 2.7 to 3.0. Next, the reaction solution was cooled to 10C or less and then a 25% sodium hydroxide aqueous solution was added to adjust to pH 7.0 to 7.5. In this reaction solution, 118.4 parts of 28% ammonia water was added and maintained at 10 to 15C and pH 9.5 to 10.0 for 3 hours. Thereafter, concentrated hydrochloric acid was added thereto to adjust to pH 6.0 to 7.0. Next, 2,000 parts of ice was added and cooled to 0C, whereto 780 parts of ethylenediamine was added dropwise while maintaining a temperature of 5C or less. Thereafter, said reaction solution was raised to 10 to 15C in temperature and maintained at the same temperature for 1 hour. Subsequently, concentrated hydrochloric acid was added dropwise thereto to adjust to pH 0.9 to 1.0. Meanwhile, the solution was maintained at 10 to 15C, while adding ice in order not to raise the temperature. Ice was further added to adjust the temperature to 10C or less. The fluid amount at this time was 13,000 parts. To this reaction solution, 2,600 parts (20% relative to the solution) of sodium chloride was added and stirred for 1 hour to precipitate a crystal. The precipitated crystal was separated by filtration and washed with 3,000 parts of a 20% sodium chloride aqueous solution to obtain 743.0 parts of a wet cake. (The concentration of the crude intended product in the wet cake: 59.3%, HPLC purity: 93.3%)
  • 2
  • [ 108-77-0 ]
  • [ 24605-36-5 ]
  • [ 81-11-8 ]
  • C32H18Cl2N10O18S6(6-)*6Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
Preparative Example 1520.2 parts of aniline-2,5-disulphonic acid monosodium salt are added to900 parts of water and dissolved with the aid of approx. 295.1 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 25 C and a pH of approx. 8 to 9. The so-formed solution is added over a period of approx. 30 minutes to331.9 parts of cyanuric chloride dispersed in 405 parts of water and 630 parts of ice. The temperature is kept below 5 C using an ice/water bath and the pH is maintained at approx. 4 to 5 using approx. 504.1 parts of an aqueous sodium carbonate solution 20 % w/w. At the end of the addition, the pH is increased to approx. 6 using approx. 35.1 parts of an aqueous sodium carbonate solution 20 % w/w and stirring is continued at approx. 0 to 5 C until completion of the reaction. 151.2 parts of sodium bicarbonate are then added to the reaction mixture. An aqueous solution, obtained by dissolving under nitrogen 333.4 parts of4,4'-diaminostilbene-2,2'-disulphonic acid in 1240 parts of water with the aid of approx. 235.8 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 45 to 50 C and a pH value of approx. 8 to 9, is dropped into the reaction mixture. The resulting mixture is stirred at approx. 45 to 50 C until completion of the reaction. The resulting aqueous mixture contains compound of formula (5) at a concentration of 0.161 mol per kg of mixture.
Example 5520.2 parts of aniline-2,5-disulphonic acid monosodium salt are added to900 parts of water and dissolved with the aid of approx. 295.1 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 25 C and a pH of approx. 8 to 9. The so-formed solution is added over a period of approx. 30 minutes to331.9 parts of cyanuric chloride dispersed in 405 parts of water and 630 parts of ice. The temperature is kept below 5 C using an ice/water bath and the pH is maintained at approx. 4 to 5 using approx. 504.1 parts of an aqueous sodium carbonate solution 20 % w/w. At the end of the addition, the pH is increased to approx. 6 using approx. 35.1 parts of an aqueous sodium carbonate solution 20 % w/w and stirring is continued at approx. 0 to 5 C until completion of the reaction.51.2 parts of sodium bicarbonate are then added to the reaction mixture. An aqueous solution, obtained by dissolving under nitrogen 333.4 parts of4,4'-diaminostilbene-2,2'-disulphonic acid in 1240 parts of water with the aid of approx. 235.8 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 45 to 50 C and a pH value of approx. 8 to 9, is dropped into the reaction mixture. The resulting mixture is stirred at approx. 45 to 50 C until completion of the reaction. The resulting aqueous mixture contains compound of formula (5) at a concentration of 0.161 mol per kg of mixture.
Example 5 520.2 parts of aniline-2,5-disulphonic acid monosodium salt are added to 900 parts of water and dissolved with the aid of approx. 295.1 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 25 C and a pH of approx. 8 to 9. The so-formed solution is added over a period of approx. 30 minutes to 331.9 parts of cyanuric chloride dispersed in 405 parts of water and 630 parts of ice. The temperature is kept below 5 C using an ice/water bath and the pH is maintained at approx. 4 to 5 using approx. 504.1 parts of an aqueous sodium carbonate solution 20 % w/w. At the end of the addition, the pH is increased to approx. 6 using approx. 35.1 parts of an aqueous sodium carbonate solution 20 % w/w and stirring is continued at approx. 0 to 5 C until completion of the reaction. 151.2 parts of sodium bicarbonate are then added to the reaction mixture. An aqueous solution, obtained by dissolving under nitrogen 333.4 parts of 4,4'-diaminostilbene-2,2'-disulphonic acid in 1240 parts of water with the aid of approx. 235.8 parts of an aqueous sodium hydroxide solution 30 % w/w at approx. 45 to 50 C and a pH value of approx. 8 to 9, is dropped into the reaction mixture. The resulting mixture is stirred at approx. 45 to 50 C until completion of the reaction. The resulting aqueous mixture contains compound of formula (5) at a concentration of 0.161 mol per kg of mixture.
  • 3
  • [ 24605-36-5 ]
  • [ 1215268-36-2 ]
  • 4
  • [ 24605-36-5 ]
  • [ 1282608-58-5 ]
YieldReaction ConditionsOperation in experiment
72% A mixture of <strong>[24605-36-5]aniline-2,5-disulfonic acid monosodium salt</strong> (8a, 13.76 g, 50 mmol) and sodium carbonate (2.8 g, 26.4 mmol) in 60 mL water was stirred to a homogeneous solution, to which was added sodium nitrite (4.0 g, 56 mmol) with vigorous stirring. The solution was stirred at 0 C for 30 min, to which was added concd HCl (10 mL) dropwise. After the precipitate of diazonium salts had appeared for 30 min, a solution of KI (10 g, 60 mmol) in H2O (10 mL) was added to the reaction mixture. After stirring for 1 h, the reaction was warmed to room temperature and then heated to 80 C to evolve nitrogen gas. When no further gas was generated, the solution was evaporated in reduced pressure to give a yellowish-orange solid 9a in 72% yield. Mp 185-186 C. 1H NMR (200 MHz, D2O) delta 8.30 (d, J = 1.8 Hz, 1H; ArH), 7.93 (d, J = 8.4 Hz, 1H; ArH), 7.72 (dd, J = 1.8, 8.4 Hz, 1H; ArH). 13C NMR (50 MHz, acetone-d6) delta 150.9, 149.9, 138.7, 128.5, 125.3, 93.3. MS (EI) m/z = 364 [M]+. Anal. (C6H5IO6S2): C, 19.79; H, 1.38. Found: C, 19.65; H, 1.30.
  • 5
  • [ 24605-36-5 ]
  • C14H16N2O6S3 [ No CAS ]
  • 6
  • [ 24605-36-5 ]
  • C12H11BrN2O4S3 [ No CAS ]
  • 7
  • [ 24605-36-5 ]
  • [ 1345020-75-8 ]
  • 8
  • [ 24605-36-5 ]
  • [ 1345020-76-9 ]
  • 9
  • [ 24605-36-5 ]
  • [ 1345020-77-0 ]
  • 10
  • [ 24605-36-5 ]
  • [ 1345020-78-1 ]
  • 11
  • [ 24605-36-5 ]
  • [ 1345020-79-2 ]
  • 12
  • [ 24605-36-5 ]
  • [ 1345020-80-5 ]
  • 13
  • [ 24605-36-5 ]
  • [ 1345020-81-6 ]
  • 14
  • [ 24605-36-5 ]
  • [ 1345020-82-7 ]
  • 15
  • [ 24605-36-5 ]
  • [ 1345020-83-8 ]
  • 16
  • [ 24605-36-5 ]
  • [ 1345020-84-9 ]
  • 17
  • [ 24605-36-5 ]
  • [ 1345020-85-0 ]
  • 18
  • [ 24605-36-5 ]
  • [ 1345020-86-1 ]
  • 19
  • [ 24605-36-5 ]
  • [ 1345020-87-2 ]
  • 20
  • [ 24605-36-5 ]
  • [ 1345020-88-3 ]
  • 21
  • [ 24605-36-5 ]
  • [ 1345020-89-4 ]
  • 22
  • [ 24605-36-5 ]
  • C12H11BrN2O4S3 [ No CAS ]
  • 23
  • [ 24605-36-5 ]
  • C12H11FN2O4S3 [ No CAS ]
  • 24
  • [ 24605-36-5 ]
  • C12H11ClN2O4S3 [ No CAS ]
  • 25
  • [ 24605-36-5 ]
  • C13H14N2O4S3 [ No CAS ]
  • 26
  • [ 24605-36-5 ]
  • C14H16N2O4S3 [ No CAS ]
  • 27
  • [ 24605-36-5 ]
  • C15H18N2O4S3 [ No CAS ]
  • 28
  • [ 24605-36-5 ]
  • C16H20N2O4S3 [ No CAS ]
  • 29
  • [ 24605-36-5 ]
  • C13H11F3N2O4S3 [ No CAS ]
  • 30
  • [ 24605-36-5 ]
  • C13H14N2O5S3 [ No CAS ]
  • 31
  • [ 24605-36-5 ]
  • C12H10F2N2O4S3 [ No CAS ]
  • 32
  • [ 24605-36-5 ]
  • C12H10Cl2N2O4S3 [ No CAS ]
  • 33
  • [ 24605-36-5 ]
  • C14H16N2O4S3 [ No CAS ]
  • 34
  • [ 24605-36-5 ]
  • C12H10Cl2N2O4S3 [ No CAS ]
  • 35
  • [ 24605-36-5 ]
  • C14H16N2O4S3 [ No CAS ]
  • 36
  • [ 24605-36-5 ]
  • [ 1345021-18-2 ]
  • 37
  • [ 108-77-0 ]
  • [ 24605-36-5 ]
  • [ 107-15-3 ]
  • [ 1035648-72-6 ]
YieldReaction ConditionsOperation in experiment
To 150 parts of ice water, 36.8 parts of cyanuric chloride and 0.4 parts of LEOCOLRTMTD-90 (trade name) were added, and this liquid was stirred at 10C or less for 30 minutes. Next, 62.0 parts of <strong>[24605-36-5]aniline-2,5-disulfonic acid monosodium salt</strong> (commercial product having a purity of 90.5%) were added thereto, and while adjusting the pH of said liquid to 2.5 to 3.0 by further adding a 10% aqueous sodium hydroxide solution, the reaction was carried out at 0 to 10C for 1 hour 30 minutes and subsequently at 20 to 25C for 1 hour 30 minutes. While adjusting to pH 9.0 to 9.5 by adding a 10% aqueous sodium hydroxide solution to the obtained reaction liquid, the reaction was carried out at 45C for 1 hour, and subsequently while likewise adjusting to pH 10.0 to 10.5, it was carried out at 45C for 1 hour. To the obtained reaction liquid, 250 parts of ice were added to cool the reaction liquid to 0C, and while adjusting so that the temperature was not over 5C, 120 parts of ethylenediamine were added dropwise to this reaction liquid. The obtained reaction liquid was stirred at room temperature overnight and then adjusted to pH 2.0 with concentrated hydrochloric acid. During the addition of concentrated hydrochloric acid, ice was added to maintain the liquid temperature at 10 to 15C. While maintaining the temperature of the resulting liquid at 50C or less, 411.0 parts of hydrochloric acid were added to adjust to pH 1.0. At this time, the liquid volume was 1200 parts. Thereto, 240 parts of sodium chloride were added, and said liquid was stirred for 30 minutes to precipitate a solid. The precipitated solid was separated by filtration to obtain 60.6 parts of a wet cake. The obtained wet cake was added to 470 parts of water, a 10% aqueous sodium hydroxide solution was added thereto to adjust to pH 10.0, whereby said wet cake was dissolved. To this solution, 33.2 parts of hydrochloric acid were added to adjust to pH 1.0. At this time, the liquid volume was 600 parts. To the resulting liquid, 120 parts of sodium chloride were added, and the mixture was stirred for 30 minutes to precipitate a solid. The precipitated solid was separated by filtration to obtain 38.4 parts of a wet cake. The obtained wet cake was added to a mixed liquid of 320 parts of methanol and 80 parts of water, said liquid was stirred at 50C for 1 hour, and then the precipitated solid was separated by filtration to obtain 38.2 parts of a wet cake. The obtained wet cake was dried to obtain 34.0 parts of a white powder of the intended organic amine for comparison represented by the above-described formula (20).
  • 38
  • [ 108-77-0 ]
  • [ 1001-53-2 ]
  • [ 24605-36-5 ]
  • [ 1426319-29-0 ]
YieldReaction ConditionsOperation in experiment
40.2 g 18.6 g of cyanuric chloride, 100 g of ice water and 4 drops of calsolene oil were added to a 2 L beaker, and the mixture was stirred at an internal temperature of 5C or less. 20.4 g of <strong>[1001-53-2]N-acetylethylenediamine</strong> was added thereto at one time at an internal temperature of 5C or less. Stirring was performed at an internal temperature of 5C for 2 hours, at room temperature overnight, at an internal temperature of 30C for 1 hour, at an internal temperature of 40C for 1 hour, and at an internal temperature of 50C for 4 hours. After the precipitated solid was filtered out while being heated, the obtained white solid was dispersed in 500 mL of acetone, and the dispersion was stirred at room temperature for 15 minutes. The solid was filtered and separated, and washed with 200 mL of acetone. The obtained white solid was dispersed in 800 mL of water at room temperature, 28.9 g of 2,5-disulfoaniline monosodium salt was added thereto, and then the pH was adjusted to 9 using a 2N sodium hydroxide [0534] aqueous solution. The internal temperature was raised to 80C, and after the reaction was performed for 2 hours, 250 g of sodium chloride was added and the temperature was lowered to room temperature. The pH was adjusted to 1 or less using concentrated hydrochloric acid, the precipitated solids were filtered out, the obtained wet cake was dispersed in 500 mL of acetone, and the dispersion was stirred at room temperature for 15 minutes. The solid was filtered out and sufficiently washed with acetone, and the obtained crystal was vacuum dried at 40C to obtain 40.2 g of a white solid. As a result of measurement of MS spectrum, 531 corresponding to [M-1]- of Intermediate B was observed.
  • 39
  • [ 24605-36-5 ]
  • [ 1426319-28-9 ]
  • 40
  • C35H30N2O4S [ No CAS ]
  • [ 24605-36-5 ]
  • C43H38N3O9S3(1-)*Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
8.2 g To 100 g of phosphorus oxychloride, 10 g of Intermediate A was added in portions, The reaction was carried out at 60 C. for 2 hours. The reaction solution was allowed to cool to room temperature, pour it into 700 g of ice water, crystals are precipitated, the precipitated crystals were separated by filtration, and washed with cold water. separately, To 300 mL of dimethylacetamide, 182.7 g of <strong>[24605-36-5]anisoline-2,5-disulfonic acid monosodium</strong> was added, It was cooled to 5 C or lower. To this, the wet cake which was filtered off as before was dividedly added so that the internal temperature does not exceed 10 C., After completion of the addition, the reaction solution was returned to room temperature,The reaction was carried out at room temperature for 6 hours.The obtained reaction solution was concentrated with a rotary evaporator,The resulting residue was purified by silica gel chromatography (packing agent: Wako gel C200 (trade name) manufactured by Wako Pure Chemical Industries, Ltd., developing solvent: chloroform / methanol = 20/1, v / v) to obtain Exemplified Compound (1-1 ) Was obtained. Yield 8.2 g.
  • 41
  • [ 675-14-9 ]
  • [ 90-20-0 ]
  • [ 26878-11-5 ]
  • [ 88-64-2 ]
  • [ 24605-36-5 ]
  • C35H26FN11O20S6 [ No CAS ]
YieldReaction ConditionsOperation in experiment
52.1% 2.75g of aniline-2,5-bis-sulfonic acid monosodium salt, dissolved in water, under the conditions of good stirring, slowly dropping 1.39g of trifluoro cyanide in -5 ~ 0 reaction 20min or so, control pH3-4, the reaction is completed After the filter, the filtrate, a shrink product;3.19 g of H acid was added to 20 mL of water to dissolve and the pH was adjusted to 4-5; a shrunken product was added dropwise to the H acid solution and incubated at 25 C in a water bath to perform a diastolic reaction. The end point was measured with Elich.2.30 g of 4-acetylamino-2-aminobenzenesulfonic acid was added to 20 mL of water, adjusted to pH 7-8 and dissolved with 0.75 g of sodium nitrite to give 4-acetylamino-2-aminobenzenesulfonic acid containing sodium nitrite.In the beaker, add a small amount of ice, then add 3mL concentrated hydrochloric acid, stirring; containing sodium nitrite 4-acetamido-2-aminobenzenesulfonic acid solution quickly into the concentrated hydrochloric acid solution in the ice bath reaction; with Congo red test paper And starch potassium iodide test paper were instantly blue; and then continue to respond for 30min, with elixir reagent detection end point; after the end of the reaction by adding sulfamic acid decomposition of excess nitrous acid, diazonium salt solution.2.54 g of 1- (4'-sulfonic acid phenyl) -3-methyl-5-pyrazolone was dissolved in 50 mL of water, adjusted to pH 7-8, and the above diazonium salt solution was added dropwise to maintain the pH 7-8 The reaction mixture was cooled to 90 C for 5 hours. After the reaction, the reaction solution was cooled to a solution of 8% sodium hydroxide in the above mixed solution, and the reaction solution was cooled to At room temperature, adjusted to pH 7-8 with concentrated hydrochloric acid to give the intermediate solution containing pyrazolone.Add about 10g of ice and 3mL concentrated hydrochloric acid in the beaker, stir well; in the above-mentioned pyrazolone-containing intermediates solution by adding 0.75g sodium nitrite dissolved, and its rapid into the concentrated hydrochloric acid solution, with Congo red Test paper and starch potassium iodide test paper were instantly blue; and then continue to respond for 30min, with elixir reagent detection end; adding sulfamic acid decomposition of excess nitrite, which was containing pyrazolone structure diazonium salt solution.The pH of the above-mentioned dichroic solution was adjusted to 7-8, and the above-mentioned solution containing the pyrazolone-containing diazonium salt was added dropwise to the shrink product to carry out the coupling reaction, and the end point was measured by the bleeding test.After the end of the reaction, the pH 7 was adjusted, and the high-light fastness azo-type red reactive dyes containing the monofluorotriazine structure was obtained by salting out, filtering and washing the filter cake and the yield was 52.1%.
  • 42
  • [ 108-77-0 ]
  • [ 90-20-0 ]
  • [ 26878-11-5 ]
  • [ 88-64-2 ]
  • [ 24605-36-5 ]
  • C35H26ClN11O20S6 [ No CAS ]
YieldReaction ConditionsOperation in experiment
58.7% Example 11.75 g of cyanuric chloride and an appropriate amount of crushed ice at 0 C with stirring; 2.75 g of aniline-2,5-bis sulfonic acid monosodium salt, 40 mL of water was added to adjust pH 6.0; aniline-2,5-bis Solution was added to the trichloro cyanide slurry to carry out a shrinkage reaction, keep the pH 4-5, reaction 3h, with elixir reagent detection end point, that was a shrink product.3.19 g of H acid was added to 20 mL of water and the pH was adjusted to 4-5. A shrunken product was added dropwise to the H acid solution and the mixture was incubated at 35 C for 35 C to maintain pH 4-5 for about 4 h. Test the end point, that is, shrink products.2.30 g of 4-acetamido-2-aminobenzenesulfonic acid was added to 20 mL of water, adjusted to pH 7-8 and dissolved with 0.75 g of sodium nitrite to give 4-acetylamino-2-aminobenzenesulfonic acid containing sodium nitrite.In the beaker, add a small amount of ice, then add 3mL concentrated hydrochloric acid, stirring; containing sodium nitrite 4-acetylamino-2-aminobenzenesulfonic acid solution quickly into the concentrated hydrochloric acid solution in the ice bath reaction, with Congo red test paper and Starch potassium iodide test paper are instantly blue.And then continue to respond for 30min, with elixir reagent detection end point; after the end of the reaction by adding sulfamic acid decomposition of excess nitrous acid, diazonium salt solution.2.54 g of 1- (4'-sulfonic acid phenyl) -3-methyl-5-pyrazolone was dissolved in 50 mL of water, adjusted to pH 7-8, and the above diazonium salt solution was added dropwise maintaining pH 7-8, The reaction solution was cooled to room temperature, and the reaction solution was cooled to room temperature. After the reaction was carried out, the reaction solution was cooled to room temperature, and the reaction solution was cooled to room temperature. The reaction solution was cooled to room temperature, Hydrochloric acid to adjust pH7-8, to obtain the structure of the intermediate containing pyrazolone solution.Add about 10 g of ice and 3 mL of concentrated hydrochloric acid in a beaker and stir the reaction in an ice bath; add 0.75 g of sodium nitrite to the solution containing the pyrazolone solution and quickly pour it into a concentrated hydrochloric acid solution and use a Congo red test paper and Starch potassium iodide test paper are instantly blue; and then continue to respond for 30min, with elixir reagent detection end point; after the end of the reaction by adding sulfamic acid decomposition reaction process generated excess nitrite, that is, the weight of the pyrazolone structure Nitrogen salt solution.Adjusting the pH of the product solution to 7-8, dropping the solution containing the pyrazolone structure diazonium salt into the shrink product to carry out the coupling reaction, detecting the end point with the bleeding experiment; adjusting the product solution pH 7, The filtrate was washed and dried to obtain high gloss fastness azo red reactive dyes containing monochlorotriazine. The yield was 58.7%.
  • 43
  • [ 108-77-0 ]
  • [ 88-63-1 ]
  • [ 24605-36-5 ]
  • [ 123-30-8 ]
  • [ 5460-09-3 ]
  • C31H18ClN10O17S5(5-)*5Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
(1) Add 100% of 19.2g of cyanuric chloride, 200g of ice and 20mL of water to a 1000mL beaker.Beating with stirring for 45 minutes, adding 100% of 18.8 g of 2,4-diaminobenzenesulfonic acid to 400 mL of water.Add sodium bicarbonate solids with stirring, adjust pH to 6 to dissolve,The solution was added dropwise to a cyanuric chloride beating solution, and the reaction conditions were controlled at 0-5 C and pH = 3-4.After 30 minutes of addition, after the addition, the reaction was continued under the conditions for 60 minutes to obtain a solution of the first condensation product of cyanuric chloride; 34.1 g of industrial hydrochloric acid (30%) was added to the solution, and stirring was continued;Add 23 g of sodium nitrite solution (30% by mass) at 5 C.The drip acceleration is based on the reaction solution to make the starch KI test paper slightly blue. After the addition is completed,The diazotization reaction was continued for 45 minutes, and Ehrlich reagent was used to detect the end point of the reaction. After the reaction is over,Excess nitrous acid is removed with sulfamic acid.(2) Add 100% of 27.5 g of aniline 2,5-disulfonic acid monosodium salt to 400 mL of water.The pH value was adjusted with baking soda under stirring, and after dissolution, 100% of 7.1 g of sodium nitrite solid was added and stirred to dissolve.The dissolved mixed solution was added to an aqueous solution of hydrochloric acid cooled to about 5 C (34.1 g of industrial hydrochloric acid (30%)Dissolved in 100mL of water), after the addition is completed, continue the diazotization reaction for 45 minutes.The Ehrlich reagent detects the end of the reaction. After the reaction is over, the excess nitrous acid is removed with sulfamic acid.Aniline2,5-disulfonic acid diazonium salt solution.(3) Add 40.1 g of monosodium salt of H acid (85%) to 400 mL of water, and add 20% NaOH solution with stirring.The pH was adjusted to 6.5, dissolved, and cooled to 5 C.The aniline 2,5-disulfonic acid diazonium salt solution prepared in the step (2) is slowly added dropwise to the solution of the H acid.Control the pH of the reaction system to about 2, keep the pH at 2, and react at a temperature of 5 C for 6 hours.The end point of the reaction was detected by the osmosis method. After the reaction was completed, the pH of the reaction system was adjusted to about 6.5 with sodium bicarbonate solid;The diazonium salt prepared in the step (1) is slowly added dropwise to the above solution, and maintained at pH=6.5.The reaction was carried out at 5 C for 4 hours;The end point of the reaction was detected by a percolation method.(4) adding 100% of 10.9 g of p-aminophenol to the H acid diazo dye prepared in the above step (3),The temperature was raised to 30 C, and the pH of the reaction system was adjusted to 6 with sodium hydrogencarbonate, and the reaction was maintained under the conditions for 2 hours.After completion of the reaction, the mixture was subjected to salting out, filtration, washing and drying to obtain a solid of the reactive dye I-1.
  • 44
  • [ 108-77-0 ]
  • [ 119-79-9 ]
  • [ 24605-36-5 ]
  • [ 123-30-8 ]
  • [ 82-75-7 ]
  • C35H20ClN9O13S4(4-)*4Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
(1) Add 100% of 27.5 g of aniline 2,5-disulfonic acid monosodium salt to 400 mL of water.Adjust the pH value 6 with baking soda under stirring, add 100% 7.1 g of sodium nitrite solid after dissolution, stir and dissolve.The dissolved mixed solution was added to an aqueous solution of hydrochloric acid cooled to about 5 C (34.1 g of industrial hydrochloric acid (30%)Dissolved in 100mL of water), after the addition is completed, continue the diazotization reaction for 45 minutes.The Ehrlich reagent detects the end of the reaction. After the reaction is over, the excess nitrous acid is removed with sulfamic acid.An aniline 2,5-disulfonic acid diazonium salt solution was obtained. Will fold 100% of 22.3g5-Amino-2-naphthalenesulfonic acid is added to the above diazonium salt solution to control the pH of the reaction to 2, and the temperature is 0-5 C.The reaction was carried out under the conditions for 6 hours, and after the reaction was completed, the pH of the system was adjusted to 6 with sodium hydrogencarbonate.A corresponding chromophore intermediate solution was prepared.(2) adding 100% of 7.1 g of sodium nitrite solid to the chromophore intermediate solution prepared in the step (1),Stir and dissolve,And the dissolved mixed solution was added to an aqueous solution of hydrochloric acid cooled to about 5 C (34.1 g of industrial hydrochloric acid (30%)Dissolved in 100 mL of water), after the addition was completed, the diazotization reaction was continued for 45 minutes.After the reaction, excess nitrous acid is removed with sulfamic acid.Preparation of the chromophore intermediate diazonium salt solution; will be 100% off 22.3g8-amino-1-naphthalenesulfonic acid is added to the above chromogenic intermediate diazonium salt solution to control the pH of the reaction to 2,The temperature is 0-5 C, and the reaction is carried out for 6 hours under the conditions, after the reaction is completed,The pH of the system was adjusted to 5 with sodium bicarbonate to prepare the corresponding chromophore solution.(3) Add 100% of 19.2g of cyanuric chloride, 200g of ice and 20mL of water to a 1000mL beaker.Beating with stirring for 45 minutes, adding 100% of 10.9 g of p-aminophenol to 400 mL of water.Add sodium bicarbonate solids with stirring, adjust pH to 7 to dissolve,The solution was added dropwise to a cyanuric chloride beating solution, and the reaction conditions were controlled at 0-5 C and pH = 5,After 30 minutes, the reaction was continued for 60 minutes under the conditions.A solution of the primary condensation product of cyanuric chloride is obtained.(4) adding the color base solution obtained in the step (2) to the step (3)The obtained first condensation product of cyanuric chloride is heated to 40 C.The pH of the system was adjusted to 5 with sodium bicarbonate, and the reaction was continued for 2 hours while maintaining the reaction conditions.After the reaction, salting out, filtering, washing and drying to obtain reactive dye III-1 solid
  • 45
  • [ 24605-36-5 ]
  • C27H19Cl2N8O9S3(1-)*Na(1+) [ No CAS ]
  • 46
  • [ 24605-36-5 ]
  • C27H21ClN9O9S3(1-)*Na(1+) [ No CAS ]
  • 47
  • [ 24605-36-5 ]
  • C24H20N5O9S3(1-)*Na(1+) [ No CAS ]
  • 48
  • [ 95-78-3 ]
  • [ 24605-36-5 ]
  • C14H13N3O6S2(2-)*2Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
(1) Add 150 ml of water to a 1000 ml beaker. Adding 19.13 g of <strong>[24605-36-5]aniline-2,5-disulfonic acid monosodium salt</strong>, Stir for 20 minutes, then adjust the pH to 7.0-7.5 with solid sodium hydroxide to completely dissolve. Stir for 30 minutes to stabilize. Add appropriate amount of ice control T = 8 ~ 12 C, continue to add 30wt% hydrochloric acid 20ml and stir for 20 minutes, then add solid sodium nitrite 5g, pay attention to control the feed rate, take the potassium iodide test paper to the blue, to prevent yellow smoke. After the addition control T=812 C, the potassium iodide starch test paper showed a blue reaction for 0.5 hours, and the excess sodium nitrite was eliminated with sulfamic acid for use. (2) adding a quantity of 8.51 g of 2,5-dimethylaniline to the above diazonium solution which has eliminated sodium nitrite, Stir the reaction for 4 hours, Process temperature control T=820C, The disappearance of diazonium salt was detected multiple times during the reaction. The diazonium salt disappeared to the end point to obtain the desired mono-but solution. (3) raising the above monolithic solution to T=53 C, And keep the monocouple solution dissolved and clarified, Then measure the volume to slow down the stirring speed, Uniform addition of 76 g of potassium chloride for salting out operation, Stir for 3 hours and take a drop of salting out into the filter paper. The hydrating ring spreads faster, and the filter cake is obtained by vacuum filtration.
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