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邻三氟甲基苯胺的合成

Synthesis of O-(Trifluoromethyl)aniline

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【作者】 刘海辉; 杜晓华; 陈静华; 徐振元;

【Author】 LIU Hai-Hui1, DU Xiao-Hua1, CHEN Jing-Hua2, XU Zhen-Yuan1(1Catalytic Hydrogenation Research Center, State Key Laboratory Breeding Base of Green Chemistry-Synthesis Technology, ZhejiangUniversity of Technology, Hangzhou 310014, China; 2Zhejiang Weihua Chemical Co., Ltd, Dongyang 322109, China)

【机构】 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; 浙江省东阳巍华化工有限公司; 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; 杭州310014; 东阳322109; 杭州310014;

【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。

【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%.

【关键词】 邻三氟甲基苯胺; 中间体; 合成;
【Key words】 o-(trifluoromethyl)aniline; intermediate; preparation;
  • 【分类号】TQ246
  • 【被引频次】6
  • 【下载频次】341
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