环酰菌胺合成工艺

Synthesis of Fenhexamid

[目的]寻找一条合成环酰菌胺的新工艺路线。[方法]以苯胺为起始原料经重氮化、偶合、还原制得中间体Ⅰ(2,3-二氯-4-羟基苯胺);再以甲基环己烷为起始原料经CO催化羰基化反应制得中间体1-甲基环己基羧酸,经酰化后得中间体Ⅲ(1-甲基环己基酰氯),中间体Ⅰ和中间体Ⅲ经缩合即得产物环酰菌胺。[结果]反应总收率为51.5%,并通过核磁和质谱对结构进行了表征。[结论]该工艺简单经济,条件温和,较适合工业化生产。

[Aims] The aim is to search for a new route for the synthesis of fenhexamid. [Methods] The intermediate I （2,3- dichloro-4-hydroxy aniline） was prepared using aniline as starting material through diazotization, coupling and reduction reaction. The intermediate II （1-methylcyclohexanecarboxylic acid） was obtained from carboxylate of methyl cyclohexane and carbon monoxide. Then the product fenhexamid was synthesized by condensation of the two intermediates. [Results] The whole yield was 51.5% and the structures were confirmed by 1H NMR and MS. [Conclusions] The process is simple, warm and economical, which is suitable for industrialized production.