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P-sulfonamide-phenylhydrazine hydrochloride and preparation process thereof

A sulfonamidophenylhydrazine and a preparation process technology, applied in the direction of sulfonamide preparation, organic chemistry, physical/chemical process catalyst, etc., can solve the problem of incomplete diazotization reaction, etc., reduce the amount of hydrochloric acid and reduce the pressure , The effect of saving the cost of the enterprise

Active Publication Date: 2017-05-10
平顶山奥思达科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process of conventional p-sulfonamidophenylhydrazine hydrochloride, the diazotization reaction is not complete, and it is easy to produce isomers of p-sulfonamidophenylhydrazine hydrochloride, but when it is used as a raw material to prepare medicines, its quality The requirements are relatively high, and the impurities shall not exceed 0.2%, so the efficiency of the diazotization reaction of sulfonamidophenylhydrazine hydrochloride needs to be improved urgently in order to obtain a purer product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of p-sulfamidophenylhydrazine hydrochloride, according to the weight ratio, the raw material for preparing this p-sulfanylhydrazine hydrochloride consists of 80 parts of p-sulfanilamide, 150 parts of hydrochloric acid, 70 parts of sodium nitrite, 60 parts of Caustic soda, 80 parts of sodium sulfite, 1 part of phase transfer catalyst and 0.1 part of strong acid catalyst; the strong acid catalyst consists of 60 parts of serpentine, 120 parts of ammonia, 40 parts of sulfuric acid and 10 parts of polyacrylamide according to the mass fraction. The catalyst is prepared before use. The specific operation is: firstly weigh the raw materials in the above proportions, calcinate the serpentine at 150-200°C for 1-2 hours, grind and pulverize the powder I, and then add ammonia water and polypropylene to the powder I. Stir and mix the amide and let it stand for 3-5h to precipitate a precipitate, then filter, wash and dry the precipitate and grind it finely to obtain powder II, ...

Embodiment 2

[0025] A kind of p-sulfamidophenylhydrazine hydrochloride, according to weight ratio, the raw material for preparing this p-sulfanilamidophenylhydrazine hydrochloride consists of 85 parts of p-aminobenzenesulfonamide, 185 parts of hydrochloric acid, 75 parts of sodium nitrite, 70 parts of Caustic soda, 85 parts of sodium sulfite, 3 parts of phase transfer catalyst and 0.2 part of strong acid catalyst; described strong acid catalyst is composed of 65 parts of serpentine, 123 parts of ammonia, 45 parts of sulfuric acid and 13 parts of polyacrylamide according to the mass fraction. The catalyst is prepared before use. The specific operation is: firstly weigh the raw materials in the above proportions, calcinate the serpentine at 150-200°C for 1-2 hours, grind and pulverize the powder I, and then add ammonia water and polypropylene to the powder I. Stir and mix the amide and let it stand for 3-5h to precipitate a precipitate, then filter, wash and dry the precipitate and grind it f...

Embodiment 3

[0033] A kind of p-sulfamidophenylhydrazine hydrochloride, according to weight ratio, the raw material of preparing this p-sulfanylaminophenylhydrazine hydrochloride consists of 90 parts of p-aminobenzenesulfonamide, 170 parts of hydrochloric acid, 80 parts of sodium nitrite, 65 parts of Caustic soda, 90 parts of sodium sulfite, 2 parts of phase transfer catalyst and 0.3 part of strong acid catalyst; described strong acid catalyst consists of 63 parts of serpentine, 125 parts of ammonia, 43 parts of sulfuric acid and 15 parts of polyacrylamide according to the mass fraction. The catalyst is prepared before use. The specific operation is: firstly weigh the raw materials in the above proportions, calcinate the serpentine at 150-200°C for 1-2 hours, grind and pulverize the powder I, and then add ammonia water and polypropylene to the powder I. Stir and mix the amide and let it stand for 3-5h to precipitate a precipitate, then filter, wash and dry the precipitate and grind it finel...

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Abstract

The invention relates to a p-sulfonamide-phenylhydrazine hydrochloride and a preparation process thereof. Raw materials for preparing the p-sulfonamide-phenylhydrazine hydrochloride comprise 80-100 parts of p-aminobenzenesulfonamide, 150-220 parts of hydrochloric acid, 70-90 parts of sodium nitrate, 60-80 parts of caustic soda, 80-100 parts of sodium sulfite, 1-5 parts of phase-transfer catalyst and 0.1-0.5 part of strong acid catalyst, wherein the strong acid catalyst comprises the following components in parts by mass: 60-70 parts of picrolite, 120-130 parts of ammonia water, 40-50 parts of sulfuric acid and 10-20 parts of polyacrylamide. According to p-sulfonamide-phenylhydrazine hydrochloride and the preparation process thereof, the addition of the strong acid catalyst increases the diazo reaction yield; the finished product has favorable quality and high purity; the waste liquid treatment pressure is relieved; and the enterprise cost is saved.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to p-sulfonamidophenylhydrazine hydrochloride and a preparation process thereof. Background technique [0002] P-sulfonamidophenylhydrazine hydrochloride is an important intermediate in the synthesis of non-steroidal anti-inflammatory drug celecoxib, which is a new type of selective COX-2 inhibitor, by selectively inhibiting COX- 2. Prevent the synthesis of prostaglandins and achieve anti-inflammatory, analgesic and antipyretic effects. Now it is widely used in the treatment of rheumatoid arthritis, rheumatoid arthritis and other diseases. In the preparation process of conventional p-sulfonamidophenylhydrazine hydrochloride, the diazotization reaction is not complete, and it is easy to produce isomers of p-sulfonamidophenylhydrazine hydrochloride, but when it is used as a raw material to prepare medicines, its quality The requirement is high, and the impurity mus...

Claims

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Application Information

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IPC IPC(8): C07C311/39C07C303/40B01J27/055
CPCB01J27/055C07C303/40C07C311/39
Inventor 白浩朱建军张兴奇
Owner 平顶山奥思达科技有限公司
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