| 碳酸二甲酯法合成N,N-二甲基苯胺的研究 |
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| 引用本文： | 刘俊峰,姜鹏,彭良福. 碳酸二甲酯法合成N,N-二甲基苯胺的研究[J]. 湖南科技大学学报(自然科学版), 2011, 0(3) |
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| 作者姓名： | 刘俊峰 姜鹏 彭良福 |
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| 作者单位： | 湖南科技大学化学化工学院; |
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| 基金项目： | 湖南省自然科学基金项目(01JJY3009) |
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| 摘 要： | 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.
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| 关 键 词： | 苯胺 N-烷基化 碳酸二甲酯 四乙基溴化铵 |
Synthesis of N,N-dimethyl anline form dimethyl carbonate |
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| LIU Jun-feng,JIANG Peng,PENG Liang-fu. Synthesis of N,N-dimethyl anline form dimethyl carbonate[J]. Journal of Hunan University of Science & Technology(Natural Science Editon), 2011, 0(3) |
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| Authors: | LIU Jun-feng JIANG Peng PENG Liang-fu |
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| Affiliation: | LIU Jun-feng,JIANG Peng,PENG Liang-fu(School of Chemistry and Chemical Engineering,Hunan University of Science and Technology,Xiangtan 411201,China) |
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| Abstract: | N-methylation of nuclephilic nitrogen in amines is a common procedure in both lab-scale and bulk-scale organic synthesis.The conventional N-Alkylation of aniline is Eschweiler-Clarke methylation.It used toxic formalin and concentrated formic acid as methylating solution.Aniline is substrate,a new way was proved that of N-alkylation by DMC catalyzed by TEAB,and the influence factor was discussed that on the result such as reaction temperature,TEAB.The best yield(93%) of N,N-dimethyl anlinewere obtained unde... |
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| Keywords: | aniline N-alkylation DMC TEAB |
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