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胺中亲核的氮原子的N-烷基化在实验室范围及批量范围有机合成中是一个非常常见的工序.传统的方法是Eschweiler-Clarke烷基化程序,采用甲酸和福尔马林进行胺的N-烷基化.提出了苯胺在碳酸二甲酯(DMC)作烷基化试剂,四乙基溴化铵(TEAB)催化下合成N,N-二甲基苯胺的新方法,讨论了物料比例、四乙基溴化铵、温度对反应结果的影响,确定了反应温度、四乙基溴化铵等的最佳用量最适宜的工艺条件是:反应温度为443 K,苯胺和碳酸二甲酯的摩尔比1∶1.2～1∶1.3,反应时间是2 h.在优选的条件下获得了产物N,N-二甲基苯胺,产率达93%,同时催化剂四乙基溴化胺得到很高的回收率.
N-alkylation of nucleophilic nitrogen atoms in amines is a very common procedure in laboratory-scale and batch-scale organic synthesis. The traditional method is the Eschweiler-Clarke alkylation procedure using formic acid and formalin Amine N-alkylation. A new method for the synthesis of N, N-dimethylaniline from aniline catalyzed by dimethyl carbonate (DMC) as tetraalkylammonium bromide (TEAB) The ratio of materials, the content of tetraethylammonium bromide, the temperature on the reaction results, to determine the reaction temperature, the optimum amount of tetraethylammonium bromide, the most suitable process conditions are: the reaction temperature is 443 K, aniline and carbonic acid Dimethyl ester molar ratio of 1: 1.2 ~ 1: 1.3, the reaction time is 2 h under the optimum conditions to obtain the product N, N- dimethylaniline, the yield was 93%, while the catalyst tetraethyl bromide Amines get high recovery.