2,6-二溴-4-三氟甲氧基苯胺合成的研究

Synthesis process of 2,6-dibromo-4-trifluoromethoxy aniline

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126 400元/t降至70 500元/t。

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-H2 02 were used as brominating agent respectively. Producthas 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-H202 as brominating agent,70 ℃,the yield is 97% and the purity of product is over 99.5%.