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Production technology of sulfanilamide intermediate acylamino benzenesulfonyl chloride

A technology of amide and benzenesulfonyl chloride, which is applied in the field of production technology of sulfonamide intermediate benzenesulfonyl chloride, can solve disadvantages and other problems, reduce waste, reduce production process and equipment investment, reduce consumption and waste acid The effect produced

Inactive Publication Date: 2019-05-24
顾一涛 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, the excess chlorosulfonic acid is not only used as a sulfonation reactant, but also used as a solvent. After the reaction, water is required to separate the excess chlorosulfonic acid after reaction treatment, thus producing a large amount of waste acid. No matter from the perspective of environmental protection or economical Angles are greatly disadvantageous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The invention provides a kind of production technology of sulfonamide intermediate amido benzenesulfonyl chloride, comprising the following steps:

[0026] (1) With acetanilide as raw material A, with alkanes, halogenated alkanes or ether organic solvents as solvent, acetanilide or formanilide is dissolved in the solvent to obtain A solution, in A solution, the mixture of raw material A and solvent The weight ratio is 1:0.5;

[0027] Described solvent is ethylene dichloride;

[0028] (2) Taking chlorosulfonic acid as raw material B;

[0029] (3) A solution and raw material B are sent into the reactor to carry out chlorosulfonation reaction of acetanilide or formanilide and chlorosulfonic acid, and the reaction temperature is 60° C., wherein the molar ratio of raw material A to raw material B is 1: 1; the reactor is a microreactor;

[0030] (4) After the reaction is finished, the reaction product and solvent are collected at the outlet of the reactor and cooled to roo...

Embodiment 2

[0032] The invention provides a kind of production technology of sulfonamide intermediate amido benzenesulfonyl chloride, comprising the following steps:

[0033] (1) Take formanilide as raw material A, use alkanes, halogenated alkanes or ether organic solvents as solvents, dissolve acetanilide or formanilide in the solvent to obtain A solution, in A solution, raw material A and solvent The weight ratio is 1:10;

[0034] Described solvent is cyclohexane;

[0035] (2) Taking chlorosulfonic acid as raw material B;

[0036] (3) A solution and raw material B are sent into the reactor to carry out chlorosulfonation reaction of acetanilide or formanilide and chlorosulfonic acid, the reaction temperature is 50° C., wherein the molar ratio of raw material A to raw material B is 1: 5; the reactor is a stirred reactor, and the rotating speed of the reactor is 100r / min;

[0037] (4) After the reaction is finished, the reaction product and solvent are collected at the outlet of the rea...

Embodiment 3

[0039] The invention provides a kind of production technology of sulfonamide intermediate amido benzenesulfonyl chloride, comprising the following steps:

[0040] (1) With acetanilide as raw material A, with alkanes, halogenated alkanes or ether organic solvents as solvent, acetanilide or formanilide is dissolved in the solvent to obtain A solution, in A solution, the mixture of raw material A and solvent The weight ratio is 1:3;

[0041] Described solvent is trichloroethane;

[0042] (2) Taking chlorosulfonic acid as raw material B;

[0043] (3) A solution and raw material B are sent into the reactor to carry out chlorosulfonation reaction of acetanilide or formanilide and chlorosulfonic acid, and the reaction temperature is 100° C., wherein the molar ratio of raw material A to raw material B is 1: 3; the reactor is a stirred reactor, and the rotating speed of the reactor is 500r / min;

[0044] (4) After the reaction is finished, the reaction product and the solvent are col...

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PUM

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Abstract

The invention belongs to the technical field of chemical synthesis and particularly relates to a production technology of a sulfanilamide intermediate acylamino benzenesulfonyl chloride. According tothe production technology, a new solvent is introduced for dissolving a raw material A, the application amount of a raw material B chlorosulfonic acid is reduced, so that the raw material B and the raw material A are subjected to a complete reaction, and the acylamino benzenesulfonyl chloride is prepared. According to the production technology, after chlorosulfonation, water does not need to be used for decomposing chlorosulfonic acid, so that the acylamino benzenesulfonyl chloride is separated out just through a small amount of water, the environment protection problem caused by waste acid inthe sulfanilamide product production process is reduced, waste of the raw material B is also reduced, the production process and equipment input are reduced, and the aim of improving the economic benefit is achieved; a micro-reactor or a pipe reactor or a high-rotation-speed stirring-type reaction kettle is used as a reactor, so that the raw material A and the raw material B are in sufficient contact, a sufficient reaction is achieved, contact of the chlorosulfonic acid and water generated through a reaction is reduced, the application amount of the chlorosulfonic acid is controlled, the waste acid amount is greatly reduced, and the environment-friendly and economical technical effect is achieved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a production process of sulfonamide intermediate amido-type benzenesulfonyl chloride. Background technique [0002] Sulfonamides are a general term for a class of drugs with the structure of p-aminobenzenesulfonamide. They have been in clinical use for decades and have a broad antibacterial spectrum. It is also convenient for long-term storage. The preparation method of sulfonamide in industrial production is to use chlorosulfonic acid to sulfonate acetanilide to obtain the intermediate product of acetaminobenzenesulfonyl chloride, which is then ammonified and hydrolyzed to finally obtain sulfonamide. In this process, excess chlorosulfonic acid is not only used as a sulfonation reactant, but also used as a solvent. After the reaction, water is required to separate the excess chlorosulfonic acid after reaction treatment, thus producing a large amount of was...

Claims

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Application Information

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IPC IPC(8): C07C303/08C07C309/88
Inventor 顾一涛陶晓春顾春俊
Owner 顾一涛
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