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Process for producing p-acetamidobenzene sulfonyl chloride

A technology for producing acetaminobenzenesulfonyl chloride and its production process, which is applied in the field of production process of acetaminobenzenesulfonyl chloride, which can solve the problems of large investment, impact of additive reaction, decomposition, deterioration, etc., so as to improve economic benefits and fill the gap in the market , to ensure the effect of stability

Inactive Publication Date: 2012-01-04
SUZHOU WUGAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Acetaminobenzenesulfonyl chloride is a pharmaceutical intermediate and the main raw material for the preparation of sulfamethoxazole and sulfathiazole and other sulfonamide drugs. At present, the domestic use is mainly for self-use, and the wet product is prepared and used immediately, otherwise it will happen. Decomposition, deterioration, and the period of reaching stable quality is only three days at most. As a real commodity, it is still blank in the market. Foreign production mainly uses cryogenic drying technology equipment and spray granulation drying to make finished products, but the additives have no effect on the reaction. influential
The development trend is that the use of cryogenic drying is beneficial to the stability of the obtained product, but the investment is relatively large

Method used

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  • Process for producing p-acetamidobenzene sulfonyl chloride
  • Process for producing p-acetamidobenzene sulfonyl chloride

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0012] In the specific example 1, the mass ratio to achieve the beneficial effect is: the mass ratio of the acetanilide:dichloroethane is 1:5.

specific Embodiment 2

[0013] In specific example 2, the mass ratio to achieve the beneficial effect is: the mass ratio of the acetanilide:dichloroethane is 1:6.

[0014] The dichloroethane solvent added is used in the dissolution process to ensure the stability of the acetaminobenzenesulfonyl chloride solution, and the finished product of acetaminophensulfonyl chloride can be guaranteed for about 180 days, which fills the gap in the market and improves economic benefit.

[0015] The main technical quality indicators of p-acetamidobenzenesulfonyl chloride:

[0016] serial number name Index value 1 Exterior White to off-white, crystalline powder 2 content ≥98% 3 moisture ≤0.5% 4 acidity ≤1.0ml / 0.1mol-NaOH / g 5 melting point 143-147℃ 6 shelf life 180 days 7 storage and transportation Temperature≤25℃; Humidity≤50%

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Abstract

The invention relates to a process for producing p-acetamidobenzene sulfonyl chloride. The process comprises: adding chlorosulfonic acid and antifebrine into acetanilide serving as a raw material to perform chlorosulfonation to obtain sulfonated oil; adding water into the obtained sulfonated oil to perform a hydrolysis reaction; subjecting the product of the hydrolysis of sulfonated oil to vacuum filtration; circularly absorbing one hydrogen chloride gas product to prepare diluted hydrochloric acid; and dissolving the other p-acetamidobenzene sulfonyl chloride product in a dissolving kettle, crystallizing, centrifuging and drying to obtain finished p-acetamidobenzene sulfonyl chloride. The process is characterized in that: dichloroethane is added in the dissolution process as a solvent, the finished product obtained after centrifugation is dried by air flow and then packed under vacuum, and thus, the finished product is obtained. In the production process disclosed by the invention, the mass ratio of the added dichloroethane solvent and the acetanilide raw material is (4-8):1, air flow is used for drying, the quality guarantee period of the prepared finished product is as long as 180 days, and the finished product is more stable.

Description

technical field [0001] The invention relates to a production process for preparing p-acetaminobenzenesulfonyl chloride from sulfonated oil. Background technique [0002] Acetaminobenzenesulfonyl chloride is a pharmaceutical intermediate and the main raw material for the preparation of sulfamethoxazole and sulfathiazole and other sulfonamide drugs. At present, the domestic use is mainly for self-use, and the wet product is prepared and used immediately, otherwise it will happen. Decomposition, deterioration, and the period of reaching stable quality is only three days at most. As a real commodity, it is still blank in the market. Foreign production mainly uses cryogenic drying technology equipment and spray granulation drying to make finished products, but the additives have no effect on the reaction. influential. The development trend is that the use of cryogenic drying is beneficial to the stability of the obtained product, but the investment is relatively large. Content...

Claims

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Application Information

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IPC IPC(8): C07C309/88C07C303/08
Inventor 施方浩
Owner SUZHOU WUGAN PHARMA
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