3-甲基-4-丁酰胺基-5-硝基苯甲酸甲酯合成方法改进

Improved method for synthesis of 4-butyrylamino-3-methyl-5-nitrobenzoate

目的:合成抗高血压药替米沙坦的重要中间体3-甲基-4-丁酰胺基-5-硝基苯甲酸甲酯。方法:以3-甲基-4-胺基苯甲酸甲酯为原料,在氯仿中与丁酰氯反应得3-甲基-4-丁酰胺基苯甲酸甲酯,将此反应液简单干燥后,直接滴入-10℃^-5℃的95%发烟硝酸中进行硝化。结果:改进了目标化合物3-甲基-4-丁酰胺基-5-硝基苯甲酸甲酯的硝化方法,两步收率达88%。结论:本方法操作简单,可实现连续放大生产,提高了收率和效率。

Obiective： To synthesize 4-butyrylamino-3-methyl-5-nitrobenzoate.Method： The methyl 4-butyrylamino-3-methylbenzoate was prepared from methyl 4-amino-3-methylbenzoate and butyryl chloride in chloroform,then the reaction solution was dropped to the 95% fuming nitric acid at-10℃～-5℃.Results： The methyl 4-butyrylamino-3-methyl-5-nitrobenzoate was prepared with overall yield of 88% using this improved synthetic procedure.Conclusion： The improved nitration method has a remarkable virtue of high yield and efficiency,and low cost;it can be used to produce continuously.