4-氨基-1-甲基-3-正丙基吡唑-5-甲酰胺合成工艺研究

以 3 正丙基吡唑 5 羧酸乙酯为起始原料 ,经多步反应合成了 4 氨基 1 甲基 3 正丙基吡唑 5 甲酰胺 ,并对工艺进行了如下改进 :(1)将甲基化、水解两步反应合并为“一勺烩”工艺 ,中间产物不需硅胶柱分离、提纯 ,直接进行水解 ;(2 )硝化后处理增加了溶媒提取工序 ;(3)还原反应采用催化还原法 ,以价廉的甲酸铵代替氯化亚硒作还原剂。总收率达到 39 3% ,较原工艺提高了8 5 % ,具有操作简单 ,反应条件温和 ,宜于工业化生产 ,为合成 4 氨基 1 甲基 3 正丙基吡唑 5 甲酰胺提供了一个较好的方法。

Synthesis of 4-Amino-1-methyl-3-n-propylpyrazole-5-carboxamide

The multistep synthesis of 4 amino 1 methyl 3 n propylpyrazole 5 carboxamide from 3 n propylpyrazole 5 carboxylic acid ethyl ester was improved as follows.(1)As the reactions of methylation and hydrolysis were completed in one reactor,the intermidiate needn't be isolated and purified by silicon colum chromatography,but was hydrolyzed directly.(2)Afertreatment with solvent extraction was added in the process of nitration.(3)Reduction reaction was conducted by catalytic reduction technology in the presence of ammonium formate and metal catalyst.The total yield was 39 3%,8 5% higher than the original technology.This method provided a better way to obtain 4 amino 1 methyl 3 n propylpyrazole 5 carboxamide and was simple,mild and more suitable for industrial production.