知识与财富的链接
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.
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%.
