Preparation method of refined sulfanilamide

A technology of sulfanilamide and chlorosulfonation, applied in the chemical industry, can solve the problems of affecting the quality of hydrochlorothiazide raw materials, reducing the purity of sulfanilamide intermediates, waste of by-products, etc., and achieving the effects of increasing yield, improving color and uniformity of the reaction system

Inactive Publication Date: 2017-11-03
HUZHOU ZHIWEI TECHNICAL SERVICE CO LTD
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

Due to the reasons of reaction temperature, time, stirring and refining in the existing chemical process route, a large number of by-products appear in the process, which not only reduces the purity of DSA intermediates, but also produces a series of waste by-products, which ultimately affects the raw material of hydrochlorothiazide The quality of the drug, causing side effects after taking it to the human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0019] A preparation method of fine sulfonamide, comprising the following steps:

[0020] ①Chlorosulfonation reaction: put chlorosulfonic acid, phosphorus trichloride, and m-chloroaniline into the reaction tank in sequence according to the molar ratio of 1:(1-3):(2-3) for chlorosulfonation reaction, the initial control The temperature is 40-50°C, and then steam heating is carried out to raise the temperature of the feed liquid to 110-120°C, and the reaction is kept for 2-3 hours;

[0021] ② Deicing: Hydraulically transfer the above materials to the high-level storage tank, and at the same time add water and ice to the deicing pot to lower the internal temperature to below 60°C;

[0022] ③ After the thawing is completed, filter most of the mother liquor, then move it to the centrifuge to filter it, and rinse it repeatedly with drinking water to make the pH value 6-7, control the water content to ≤ 20%, and obtain a gray-green to gray-yellow product. Chlorosulfonate wet product...

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PUM

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Abstract

The invention discloses a preparation method of refined sulfonamide, which is characterized in that it comprises the following steps: (1) chlorosulfonation reaction; (2) deicing; (3) rejection filtration on a centrifuge; (4) amination reaction; (5) refining decolorization. The preparation method of a kind of fine sulfonamide of the present invention, adds cuprous chloride catalyst in chlorosulfonation reaction, and optimizes existing process step, effectively reduces raw material feeding ratio, reduces the generation of by-product and post-treatment, and through improving amine Compound dissolution decolorization and crystallization purification process greatly improves the purity of the produced product, and its main component content can reach more than 99.5%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of sulfonamide. Background technique [0002] At present, there are few reports on the synthetic process of fine sulfonamide at home and abroad. The industry generally adopts m-chloroaniline as the starting material, and synthesizes fine sulfonamide through steps such as chlorosulfonation, deglazing, amination, and refining, and the chlorine obtained by the chlorosulfonation reaction Ammonia (NH3) is introduced into the sulfonate for amination reaction to obtain the crude refined sulfonamide. Due to the reasons of reaction temperature, time, stirring and refining in the existing chemical process route, a large number of by-products appear in the process, which not only reduces the purity of DSA intermediates, but also produces a series of waste by-products, which ultimately affects the raw material of hydrochlorothiazide The quality of the medici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/38C07C303/44C07C311/39
CPCC07C303/38C07C303/08C07C303/44C07C311/39C07C309/88
Inventor 陈丽莎
Owner HUZHOU ZHIWEI TECHNICAL SERVICE CO LTD
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