芳基吡唑腈的合成工艺研究

Synthesis of N-Phenylpyrazolecarbonitrile

以2,6-二氯-4-三氟甲基苯胺和2,3-二氰基丙酸乙酯为原料合成了氟虫腈主要中间体芳基吡唑腈。研究确定的关环反应的小试优惠条件为:18g偶氮中间体溶于40mL二氯甲烷,再加浓氨水30mL,于10℃下搅拌3h。采用该工艺路线操作简单,易于工业化,且减少了废酸的处理和高毒性试剂的使用,收率达91.4%。

N-Phenylpyrazolecarbonitrile, an important intermediate of insecticide fipronil, was synthesized from 2,6- dichloro-4-trifluoromethylaniline and 2,3-dicyanopropionate . The appropriate reaction conditions are found as follows： 30 mL of aqueous ammonia was added to a mixture of 18 g unpurified azo intermediate in 40 mL dichloromethane, and the mixture was agitated at 10℃ for 3 hours. The new method has a characteristic of simple operation, applicable industrialization, low waste acid amount less use of high toxicity reagents.