摘要
以4-三氟甲基苯胺、浓盐酸、双氧水为起始原料合成2,6-二氯-4-三氟甲基苯胺,2,6-二氯-4-三氟甲基苯胺再和2,3-二氰基丙酸乙酯反应合成中间体芳基吡唑腈,5-氨基-3-氰基-1-(2,6-二氯-4-三氟甲基-苯基)吡唑经过硫氰化、缩合、催化氧化合成目标化合物氟虫腈。重点讨论了反应时间、温度、投料比对2,6-二氯-4-三氟甲基苯胺和5-氨基-3-氰基-1-(2,6-二氯-4-三氟甲基-苯基)吡唑收率的影响。采用该工艺操作简单,易于工业化,且减少了废酸的处理和高毒性试剂的使用。
2,6-dichloro-4-trifluoromethylaniline was synthesized by using 4 trifluoromethylaniline,as starting material. N-phenylpyrazolecarbonitrile was synthesized from 2,6-dichloro-4-trifluoromethylaniline 2,3-dicyanopropinate. The effects of the reaction time , temperature and the molar ratio of hydrogen peroxide to 4-trifluoromethylaniline and N-phenylpyrazolecarbonitrile The new method has a characteristic of simple operation. Applicable industrialization, low waste acid, amount less use of high toxicity reagents.