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Method for preparing sulfadoxine

A technology of cycle-acting sulfonamide and aminobenzenesulfonamide group is applied in the field of preparing cycle-acting sulfonamide, which can solve the problems of high heat and unstable reaction, and achieve the effect of stable reaction and lower heat.

Inactive Publication Date: 2015-03-25
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the existing method for preparing sulfonamide, the heat emitted by the reaction is high, and the reaction is not stable enough

Method used

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Examples

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Embodiment Construction

[0009] The specific implementation of the present invention will be further described below in conjunction with the examples. The following examples are only used to illustrate the technical solution of the present invention more clearly, but not to limit the protection scope of the present invention.

[0010] The technical scheme of concrete implementation of the present invention is:

[0011] A method for preparing sulfonamides, comprising the steps of:

[0012] 1) Put the trichlorethylene solution of 4-(p-aminobenzenesulfonamido)-5-methoxy-6-chloropyrimidine into the reaction vessel, then add sodium hydroxide and water, stir for 30 minutes, then add methanol, and heat up Reflux reaction at 75°C for 3.5 hours to form a mixture;

[0013] 2) Distill the mixture at 85°C to remove methanol, raise the temperature to 120°C to remove trichlorethylene, then add hydrochloric acid, adjust the pH value to 9.1, then add activated carbon and stir for decolorization for 2.5 hours to obt...

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PUM

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Abstract

The invention discloses a method for preparing sulfadoxine. The method comprises the following steps: 1) inputting a trichloro ethylene solution of 4-(p-amino benzenesulfonamido)-5-methoxyl-6-chloropyrimidin into a reaction container, then adding sodium hydroxide and water, stirring for 30 minutes, then adding methanol, and heating to 75 DEG C for reflux reaction for 3.5 hours to form a mixture; 2) distilling the mixture at 85 DEG C to remove methanol, raising the temperature to 120 DEG C and distilling to remove trichloro ethylene, then adding hydrochloric acid, adjusting the pH value to 9.1, and then adding active carbon to stir and decolor for 2.5 hours to obtain a clean liquid; and 3) raising the temperature of the clean liquid to 65 DEG C, titrating a 45% glacial acetic acid solution, adjusting the pH value to 4.7, precipitating and centrifugalizing and dehydrating to obtain the sulfadoxine. The method for preparing sulfadoxine disclosed by the invention can be used for effectively reducing heat emitted by reaction, so that the reaction is stably carried out.

Description

technical field [0001] The invention relates to a method for preparing sulfonamide. Background technique [0002] In the existing method for preparing sulfonamide, the heat emitted by the reaction is high, and the reaction is not stable enough. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing sulfonamide, which can effectively reduce the heat emitted by the reaction, so that the reaction can proceed smoothly. [0004] In order to achieve the above object, technical scheme of the present invention is to design a kind of method for preparing sulfonamide, comprising the steps: [0005] 1) Put the trichlorethylene solution of 4-(p-aminobenzenesulfonamido)-5-methoxy-6-chloropyrimidine into the reaction vessel, then add sodium hydroxide and water, stir for 30 minutes, then add methanol, and heat up Reflux reaction at 75°C for 3.5 hours to form a mixture; [0006] 2) Distill the mixture at 85°C to remove methanol, rai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 李涛
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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