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邻三氟甲基苯胺的合成
引用本文:刘海辉,杜晓华,陈静华,徐振元.邻三氟甲基苯胺的合成[J].农药,2005,44(10):464-465,470.
作者姓名:刘海辉  杜晓华  陈静华  徐振元
作者单位:1. 浙江工业大学催化加氢研究中心、绿色化学合成技术国家重点实验室培育基地,杭州,310014
2. 浙江省东阳巍华化工有限公司,东阳,322109
摘    要:以邻甲基苯胺为起始原料,先与双(三氯甲基)碳酸酯反应制得邻甲基苯基异氰酸酯,然后在过氧化物催化下侧链氯化得邻三氯甲基苯基异氰酸酯,最后在无水氟化氢中同时进行氟化和溶解得邻三氟甲基苯胺,三步总收率为55.3%,产品纯度在99%以上.此路线原料易得、操作安全、分离简单、产品纯度高,是一条可行的工业化路线.

关 键 词:邻三氟甲基苯胺  中间体  合成
文章编号:1006-0413(2005)10-464-03
收稿时间:2005-02-03
修稿时间:2005-02-032005-03-28

Synthesis of O-(Trifluoromethyl)aniline
LIU Hai-Hui,DU Xiao-Hua,CHEN Jing-Hua,XU Zhen-Yuan.Synthesis of O-(Trifluoromethyl)aniline[J].Pesticides,2005,44(10):464-465,470.
Authors:LIU Hai-Hui  DU Xiao-Hua  CHEN Jing-Hua  XU Zhen-Yuan
Affiliation:1.Catalytic Hydrogenation Research Center, State Key Laboratory Breeding Base of Green Chemistry-Synthesis Technology, Zhejiang University of Technology, Hangzhou 310014, China; 2.Zhejiang Weihua Chemical Co., Ltd, Dongyang 322109, China
Abstract:An operationally safe and separately simple process was described for the preparation of o-(trifluoromethyl)aniline. Firstly, o-Toluidine as the starting material reacted with bis(trichloromethyl)carbonate to give o-tolylisocyanate.Secondly, o-tolylisocyanate was chlorinated in the presence of a peroxide to give o-(trichloromethyl)phenyl isocyanate.Finally, o-(trichloromethyl)phenyl isocyanate was fluorinated and solvolyzed in anhydrous hydrogen fluoride in one pot to yield thetitled compound o-(trifluoromethyl)aniline. The total yield was 55.3% and the purity of the product was above 99%.
Keywords:o-(trifluoromethyl)aniline  intermediate  preparation
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