Method for preparing aceclofenac

Abstract

The invention discloses a preparation process of novel aceclofenac. The preparation process of novel aceclofenac which is stated by the invention comprises filling diclofenac and toluene in a reaction bottle, stirring under the condition of outside temperature, dripping triethylamine until the solution is clarified, dripping tert-butyl bromoacetate to react for 3-4 hours when temperature is 50-60 DEG C, dripping 30% NaOH solution to alkalize after reaction, separating layers, scouring organic layer with water, drying with anhydrous sodium sulfate, filtering, steaming out organic solvent, dripping formic acid, reacting for 1 hour with 56-60 DEG C, dripping pure water when temperature is 0-5 DEG C, crystallizing for two hours, filtering and drying to obtain aceclofenac crystal (mp.151-152 DEG C). The process utilizes the advantages that tert-butyl is easy to be removed without the catalysis of palladium-charcoal and hydrogenization reaction, and tert-butyl is removed under the action of formic acid to obtain aceclofenac. The reaction can be conducted under smooth condition, which firstly improves reaction condition, secondly reduces environment pollution, and thirdly increases product yield.

Description

technical field [0001] The invention relates to a new preparation method of aceclofenac. Background technique [0002] Aceclofenac is an anti-inflammatory and analgesic drug that has been used in clinical treatment in recent years. Because of its strong anti-inflammatory and analgesic properties and few gastrointestinal side effects of conventional anti-inflammatory and analgesic effects, the amount of clinical use is increasing, but its synthesis The process is relatively traditional, mostly diclofenac and benzyl bromoacetate react to generate aceclofenac benzyl, and then, under the catalysis of palladium carbon, debenzylate through hydrogenation to obtain aceclofenac. [0003] The purpose of this invention is to provide a kind of new preparation method of aceclofenac. Diclofenac and tert-butyl bromoacetate are reacted to generate aceclofenac tert-butyl, which can be removed under the action of formic acid without palladium-carbon catalysis and hydrogenation reaction to ob...

AI Technical Summary

Problems solved by technology

[0002] Aceclofenac is an anti-inflammatory and analgesic drug that has been used in clinical treatment in recent years. Because of its strong anti-inflammatory and analgesic properties and few gastrointestinal side effects of conventional anti-inflammatory and analgesic effects, the amount of clinical use is increasing, but its synthesis The process is relatively traditional, mostly diclofenac and benzyl bromoacetate react to form aceclofenac benzyl, and then under the catalysis of palladium carbon, debenzylate by hydrogenation reaction to obtain aceclofenac