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Preparation method of intermediate of non-steroidal anti-inflammatory drug

A technology for intermediates and compounds, which is applied in the field of preparation of non-steroidal anti-inflammatory drug nimesulide, can solve the problems of polluted air, bad smell of pyridine, long preparation time, etc., and achieves saving reaction time, shortening reaction steps, Avoid the effects of recrystallization

Inactive Publication Date: 2010-07-07
天津益倍信生物工程有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has long preparation time, many reaction steps, high cost, and pyridine has a foul smell, pollutes the air, and cannot meet the requirements of industrialized large-scale production, so it is necessary to improve this method

Method used

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Examples

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Effect test

Embodiment 1

[0009] Example 1. In a three-necked flask equipped with mechanical stirring and a drying tube of 3 L, add 10 L of ethyl acetate solution containing 1300 g of o-aminodiphenyl ether, add 831 g of methanesulfonyl chloride dropwise at 80° C., and react for 2 hours. Cool, stir, filter and dry to obtain 2-phenoxymethanesulfonanilide. The yield was 85%.

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PUM

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Abstract

The invention relates to a preparation method of an intermediate of a non-steroidal anti-inflammatory drug, in particular to the preparation method of a nimesulide intermediate of 2-phenoxy-methane-sulfonyl aniline. The preparation method of the nimesulide intermediate of the 2-phenoxy-methane-sulfonyl aniline comprises the following steps: adding o-amino diphenyl ether (I) into a reactor which is provided with a drying and condensing device, adding an organic solvent, continuously adding methanesulfonyl chloride within one hour of heating, filtering and drying mixture, and obtaining 2-phenoxy methanesulfonyl chloride (II).

Description

technical field [0001] The invention relates to a preparation method of a non-steroidal anti-inflammatory drug nimesulide, more specifically a preparation method of a nimesulide intermediate 2-phenoxymethanesulfonanilide. Background technique [0002] Nimesulide is a new type of non-steroidal anti-inflammatory drug with antipyretic and analgesic activity. The preparation method of the disclosed compound (II) is to add methanesulfonyl chloride to the pyridine solution of o-aminodiphenyl ether within three hours, then pour into 5L ice and 2L concentrated hydrochloric acid mixed solution, filter, and wash with 100% hydrochloric acid The crude product 2-phenoxymethanesulfonanilide was recrystallized from a mixture of ethanol and water. This method has long preparation time, many reaction steps, high cost, and pyridine has a foul smell, pollutes the air, and cannot meet the requirements of industrialized large-scale production. Therefore, it is necessary to improve this method. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/08C07C303/38
Inventor 崔景柏
Owner 天津益倍信生物工程有限责任公司
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