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Efficient catalytic preparation method for acetamidobenzenesulfony chloride

A technology for the preparation of acetaminobenzenesulfonyl chloride and catalysis, which is applied to the preparation of sulfonic acid, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of less reaction by-products, large amount of chlorosulfonic acid, and inconvenient disposal of waste acid. , to achieve the effect of reducing acidity, improving purity and practicality

Inactive Publication Date: 2019-08-23
新乡市锦源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies in the prior art, the present invention provides a high-efficiency catalytic preparation method for acetaminobenzenesulfonyl chloride, which has the advantages of less chlorosulfonic acid consumption, less reaction by-products and the ability to recycle waste, and solves the problem of previous processes. The problem of excessive consumption of chlorosulfonic acid in the process, inconvenient disposal of waste acid and high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A high-efficiency catalytic preparation method for acetaminobenzenesulfonyl chloride, comprising the following steps: firstly adding the reaction solvent chloroform into the reaction kettle, and then adding acetanilide and chlorosulfonic acid into the chlorosulfonation reaction kettle in proportion from two different directions Among them, both sides of the chlorosulfonation reaction kettle are provided with material inlet pipes, and one side of the material inlet pipe is provided with a solvent pump. The two material inlet pipes are placed obliquely, and their axes meet in the chlorosulfonation reaction kettle In the center of the center, acetanilide is passed into one of the material inlet pipes, and chlorosulfonic acid is passed into the other material inlet pipe, and pressurized atomization treatment is carried out during the addition process, and the pressure range is 0.15; the mixed solution is stirred, and the stirring time is for 1h; then the reaction solution is...

Embodiment 2

[0026] A high-efficiency catalytic preparation method for acetaminobenzenesulfonyl chloride, comprising the following steps: firstly adding the reaction solvent chloroform into the reaction kettle, and then adding acetanilide and chlorosulfonic acid into the chlorosulfonation reaction kettle in proportion from two different directions Among them, both sides of the chlorosulfonation reaction kettle are provided with material inlet pipes, and one side of the material inlet pipe is provided with a solvent pump. The two material inlet pipes are placed obliquely, and their axes meet in the chlorosulfonation reaction kettle In the center of the center, acetanilide is passed into one of the material inlet pipes, and chlorosulfonic acid is passed into the other material inlet pipe, and pressurized atomization treatment is carried out during the addition process, and the pressure range is 0.2MP; the mixed solution is stirred and stirred. The time is 1.5h; then the reaction solution is h...

Embodiment 3

[0029] A high-efficiency catalytic preparation method for acetaminobenzenesulfonyl chloride, comprising the following steps: firstly adding the reaction solvent chloroform into the reaction kettle, and then adding acetanilide and chlorosulfonic acid into the chlorosulfonation reaction kettle in proportion from two different directions Among them, both sides of the chlorosulfonation reaction kettle are provided with material inlet pipes, and one side of the material inlet pipe is provided with a solvent pump. The two material inlet pipes are placed obliquely, and their axes meet in the chlorosulfonation reaction kettle In the center of the center, acetanilide is passed into one of the material inlet pipes, and chlorosulfonic acid is passed into the other material inlet pipe, and pressurized atomization treatment is carried out during the addition process, and the pressure range is 0.25MP; the mixed solution is stirred and stirred. The time is 2 hours; then the reaction solution ...

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Abstract

The invention relates to the technical field of chemical intermediate synthesis and discloses an efficient catalytic preparation method for acetamidobenzenesulfony chloride. The efficient catalytic preparation method comprises the following steps: firstly, putting a reaction solvent chloroform into a reaction kettle; and secondly, respectively putting acetanilide and chlorosulfonic acid into the chlorosulfonation reaction kettle from two different directions in a ratio, wherein material inlet tubes are arranged on both sides of the chlorosulfonation reaction kettle. According to the efficientcatalytic preparation method for acetamidobenzenesulfony chloride, the acetanilide and the chlorosulfonic acid are subjected to vacuum atomization treatment at an early reaction stage, and stirring isimplemented, so that the sulfonation process can be accelerated, and the reaction efficiency is improved; in addition, phosphorus pentachloride is added in a later reaction process, and a chlorination reaction is implemented, so that the amount of waste liquids in a chlorosulfonic acid reaction process is reduced; and due to adoption of calcium chloride, the content of chloride ions in the reaction process is greatly increased, and reactions are promoted towards generation of the acetamidobenzenesulfony chloride.

Description

technical field [0001] The invention relates to the technical field of synthesis of chemical intermediates, in particular to a highly efficient catalytic preparation method of acetaminobenzenesulfonyl chloride. 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 to achieve stable quality is only three days at most. As a real commodity, it is still blank in the market. Overseas production mainly adopts cryogenic drying technology equipment and spray granulation drying to make finished products, but additives have an impact on the reaction. The development trend is that the use of cryogenic drying is beneficial to the stability of the obtained pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/88C07C303/08C07C303/44
CPCC07C303/08C07C303/44C07C309/88
Inventor 闫玲玲蔡红新陈亮陈东梅张国祥刘媛媛
Owner 新乡市锦源化工有限公司