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Method for synthesizing high-purity sulfanilamide by taking acetanilide as raw material and sulfanilamide

An acetanilide and high-purity technology, applied in the field of p-aminobenzenesulfonamide synthesis, can solve the problems of low yield and purity, and achieve the effects of high content, high purity and high purity

Inactive Publication Date: 2018-09-21
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

Adopt chlorosulfonic acid p-acetanilide to carry out chlorosulfonation reaction in the prior art, because this reaction is an equilibrium reaction, even if adopting a large amount of and excessive chlorosulfonic acid to participate in the reaction, there are still 20% p-acetanilides that cannot be converted Become p-acetylaminobenzenesulfonyl chloride, resulting in low yield and purity of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of method that takes acetanilide as raw material synthetic high-purity sulfanilamide, comprising:

[0041] S1. Mix acetanilide with a mass ratio of 1:3.5 and glacial acetic acid in a reaction kettle to obtain a reaction stock solution. Under the action of ultraviolet light, heat the reaction stock solution to 65°C, stir at a speed of 500r / min, pass dry air into the reaction stock solution until the pressure in the reaction kettle reaches 0.25MPa, stop passing the dry air and then inject it into the reaction stock solution at the same time Feed sulfur dioxide gas and chlorine gas until the pressure inside the reactor reaches 0.5MPa, then simultaneously feed sulfur dioxide gas, chlorine gas and oxygen into the reaction stock solution until the pressure inside the reactor reaches 0.75MPa, then stop the external ventilation and ventilate the inside air of the reactor Into the reaction stock solution and continue to react for 4h. Glacial acetic acid was recovered under...

Embodiment 2

[0046] A kind of method that takes acetanilide as raw material synthetic high-purity sulfanilamide, comprising:

[0047] S1. Mix acetanilide with a mass ratio of 1:3 and glacial acetic acid in a reaction kettle to obtain a reaction stock solution. Under the action of ultraviolet light, heat the reaction stock solution to 60°C, stir at a speed of 400r / min, pass dry air into the reaction stock solution until the pressure in the reaction kettle reaches 0.2MPa, stop passing the dry air and then inject it into the reaction stock solution at the same time Feed sulfur dioxide gas and chlorine gas until the pressure inside the reactor reaches 0.5MPa, then simultaneously feed sulfur dioxide gas, chlorine gas and oxygen into the reaction stock solution until the pressure inside the reactor reaches 0.7MPa, then stop the external ventilation and ventilate the inside air of the reactor Into the reaction stock solution and continue to react for 4.5h. Glacial acetic acid was recovered under...

Embodiment 3

[0052] A kind of method that takes acetanilide as raw material synthetic high-purity sulfanilamide, comprising:

[0053] S1. Mix acetanilide with a mass ratio of 1:4 and glacial acetic acid in a reaction kettle to obtain a reaction stock solution. Under the action of ultraviolet light, heat the reaction stock solution to 70°C, stir at a speed of 600r / min, pass dry air into the reaction stock solution until the pressure in the reactor reaches 0.3MPa, stop passing the dry air, and then inject it into the reaction stock solution at the same time Feed sulfur dioxide gas and chlorine gas until the pressure inside the reactor reaches 0.5MPa, then simultaneously feed sulfur dioxide gas, chlorine gas and oxygen into the reaction stock solution until the pressure inside the reactor reaches 0.8MPa, then stop the external ventilation and ventilate the inside air of the reactor Into the reaction stock solution and continue to react for 3.5h. Glacial acetic acid was recovered under reduce...

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Abstract

The invention provides a method for synthesizing high-purity sulfanilamide by taking acetanilide as a raw material and the sulfanilamide and belongs to the field of synthesis of sulfanilamide. The method comprises the following steps: mixing acetanilide and glacial acetic acid to obtain a reaction stock solution; meanwhile, introducing sulfur dioxide gas and chlorine gas into the reaction stock solution under the action of ultraviolet irradiation and under the condition of stirring and heating at 60 to 70 DEG C; carrying out chlorosulfonation reaction, and decompressing and recycling glacial acetic acid to obtain sulfanilamide. Sulfanilamide is subjected to amination reaction and hydrolysis reaction in sequence. The method is simple to operate and the purity of prepared sulfanilamide is high.

Description

technical field [0001] The invention relates to the field of synthesis of p-aminobenzenesulfonamide, and in particular to a method for synthesizing high-purity p-aminobenzenesulfonamide by using acetanilide as a raw material and p-aminobenzenesulfonamide. Background technique [0002] In addition to being used to prepare crystalline sulfonamide for external anti-inflammation, p-aminobenzenesulfonamide can also be used to synthesize other sulfa drugs such as sulfamidine, sulfamethoxazine, sulfamethazine, etc. It is an important medicine and intermediate. [0003] At present, it is a common route to synthesize p-aminobenzenesulfonamide from acetanilide as a raw material. Adopt chlorosulfonic acid p-acetanilide to carry out chlorosulfonation reaction in the prior art, because this reaction is an equilibrium reaction, even if adopting a large amount of and excessive chlorosulfonic acid to participate in the reaction, there are still 20% p-acetanilides that cannot be converted B...

Claims

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Application Information

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IPC IPC(8): C07C311/39C07C303/40C07C303/38C07C311/46C07C303/10C07C309/88
CPCC07C303/10C07C303/38C07C303/40C07C311/39C07C309/88C07C311/46
Inventor 闫玲玲蔡红新魏艳军王永强张国祥
Owner 新乡市锦源化工有限公司
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