2,6-二溴-4-三氟甲氧基苯胺合成的研究

摘要

A synthesis process of 2,6-dibromo-4-trifluoromethoxy aniline, which came from 4-triflu-oromethoxy aniline was described. Different reaction temperature was selected as room temperature, 40,60 and 70℃. Furthermore,Br2 and Br2-H2O2 were used as brominating agent respectively. Product has been confirmed by the data of m. p. , IR, UV,1H-NMR, ESI-MS. The purity of product is determined by HPLC &- UPLC. The results showed that the best conditions are as follows, water-soluble, Br2-H2O2 as brominating agent,70 ℃ ,the yield is 97% and the purity of product is over 99. 5%.%研究了对三氟甲氧基苯胺溴代制备2,6-二溴-4-三氟甲氧基苯胺的各种工艺条件,考察了溶剂、反应温度、溴化试剂对反应的影响,并用IR、UV、1 H-NMR、ESI-MS对目标产物结构进行了表征,并用 HPLC 及 UPLC 检测了产品纯度.结果表明,在水溶剂中、70℃下使用液溴-双氧水作溴化试剂,收率可达97％以上,纯度达99.5％以上.经工艺优化将目标产品的原料成本从126400元/t降至70500元/t.