文献类型：期刊文献

中文题名：2-甲硫基-4-三氟甲基苯甲酸甲酯的合成

英文题名：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：[1]华东理工大学药学院,上海200237

年份：2013

卷号：52

期号：6

起止页码：402

中文期刊名：农药

外文期刊名：Agrochemicals

收录：CSTPCD;;北大核心:【北大核心2011】；CSCD:【CSCD_E2013_2014】；

语种：中文

中文关键词：2-甲硫基-4-三氟甲基苯甲酸甲酯;异噁唑草酮;除草剂;合成

外文关键词：methyl 2-methylthio-4-（trifluoromethyl）benzoate; isoxaflutole; herbicide; synthesis

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.