Method of preparing orthotrifluoromethyl aniline
    1.
    发明授权
    Method of preparing orthotrifluoromethyl aniline 失效
    正三氟甲基苯胺的制备方法

    公开(公告)号:US4387246A

    公开(公告)日:1983-06-07

    申请号:US328067

    申请日:1981-12-07

    摘要: A process for preparing orthotrifluoromethyl aniline from trifluoromethyl benzene is disclosed. The steps are (a) reacting the trifluoromethyl benzene with gaseous chlorine in the presence of a chlorination catalyst until at least 90% of the trifluoromethyl benzene is consumed; (b) nitrating the crude mixture from step (a) using a mixture of sulfuric acid and nitric acid until disappearance of the chlorotrifluoromethyl benzenes; (c) settling and washing the organic phase from step (b); (d) subjecting the organic phase from step (c) to a first hydrogenation under pressure in the presence of a hydrogenation catalyst consisting of Raney nickel and/or Raney nickel doped with chromium, in an organic-solvent medium until complete disappearance of the chloronitrotrifluoromethyl benzenes; (e) subjecting the mixture from step (d) to a second hydrogenation in the presence of an additional amount of Raney nickel and in the presence of at least one alkaline base; and (f) removing the orthotrifluoromethyl aniline by distillation from the reaction mixture.

    摘要翻译: 公开了一种由三氟甲苯制备邻三氟甲基苯胺的方法。 步骤是(a)在氯化催化剂的存在下使三氟甲基苯与气态氯反应,直到三氟甲基苯的至少90%被消耗; (b)使用硫酸和硝酸的混合物硝化来自步骤(a)的粗混合物,直至氯三氟甲苯苯消失; (c)沉淀并洗涤步骤(b)的有机相; (d)在有机溶剂介质中,在有机溶剂介质中,在由含有铬的阮内镍和/或阮内镍组成的氢化催化剂的存在下,在压力下使步骤(c)的有机相进行第一次氢化,直到氯三氟甲基甲基 苯; (e)使来自步骤(d)的混合物在额外量的阮内镍存在下并在至少一种碱性碱的存在下进行第二次氢化; 和(f)通过蒸馏从反应混合物中除去邻三氟甲基苯胺。