2-甲硫基-4-三氟甲基苯甲酸甲酯的合成  

The Synthesis of Methyl 2-Methylthio-4-(trifluoromethyl)benzoate

作　　者：牛纪凤[1] 廖道华[1] 汤阿萍[1] 解西军[1] 高倩[1] 李爱军[1] 

机构地区：[1]华东理工大学药学院,上海200237

出　　处：《农药》2013年第6期402-404,407,共4页Agrochemicals

摘　　要：[目的]旨在优化合成2-甲硫基-4-三氟甲基苯甲酸甲酯,并寻找一条适用于工业化生产的工艺路线。[方法]以对溴三氟甲苯为原料,首先进行硝化,然后经2步取代分别以氰基和甲硫基取代溴和硝基,得到2-甲硫基-4-三氟甲基苯腈,再水解,最后酯化得到目标中间体2-甲硫基-4-三氟甲基苯甲酸甲酯。[结果]反应总收率为56.5%,2-甲硫基-4-三氟甲基苯甲酸甲酯含量为98.2%(HPLC),所有中间体及产物经MS或1H NMR等进行表征。[结论]该路线条件温和、操作简便、收率较高,为工业化生产奠定了基础。[Aims] This article aims to obtain a reasonable route of methyl 2-methylthio-4-（trifluorgmethyl）benzoate on industrial scale. [Methods] Methyl 2-methylthio-4-（trifluoromethyl）benzoate was synthesized from 2-bromo-4- （trifluoromethyl）benzene via five steps including nitration, cyano substitution, methylthio substitution, hydrolysis and esterification. [Results] The total yield was 56.5%, and the purity of methyl 2-methylthio-4-（trifluoromethyl）benzoate was 98.2%（HPLC）. The products and intermediates were determined by ~H NMR or MS and so on. [Conclusions] The rout has advantages of easily available raw materials, high yield, simple operation and mild conditions, which lays the groundwork for industrial production.

关 键 词：2-甲硫基-4-三氟甲基苯甲酸甲酯 异噁唑草酮 除草剂 合成 

分 类 号：TQ457.2[化学工程—农药化工]