芳基吡唑腈的合成工艺研究  

Synthesis of N-Phenylpyrazolecarbonitrile

作　　者：陈震[1] 曹晓群[1] 王玉民[1] 张昌军[1] 林晓辉[1] 

机构地区：[1]泰山医学院化学与化学工程学院,山东泰安271016

出　　处：《精细化工中间体》2007年第3期30-31,66,共3页Fine Chemical Intermediates

基　　金：泰安市科技发展计划项目(20061023)。

摘　　要：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.

关 键 词：氟虫腈 芳基吡唑腈 合成 杂环 

分 类 号：TQ252.1[化学工程—有机化工]