3,5,6-三氯吡啶-2-醇钠的工艺优化  

Process Optimization of 3,5,6-Trichloropyridin-2-ol Sodium

作　　者：陈芳[1] 高忠良[1] 耿丽[1] 杜晓宇[1] 牛彬波 刘伟[1] 

机构地区：[1]河北工业大学化工学院,天津300130

出　　处：《化学世界》2015年第10期605-608,共4页Chemical World

摘　　要：3,5,6-三氯吡啶-2-醇钠是合成杀虫剂毒死蜱的重要中间体。以三氯乙酰氯、丙烯腈为原料,邻二氯苯为溶剂,氯化亚铜和铜粉作催化剂经加成环化、芳构化,得到3,5,6-三氯吡啶-2-醇钠(以下简称三氯吡啶醇钠)。实验对溶剂的选择、丙烯腈的加料方式、回流方式、催化剂套用、原料的重复使用等反应条件进行了考察,得出以邻二氯苯为溶剂,丙烯腈一次性加入,回流液回流到液面以下,催化剂可重复套用十次,原料经过精馏可重复使用的考察结果,使其在工业生产上操作更便利,同时最终总收率可达84.1%。3,5,6-Trichloropyridin-2-ol sodium is an important intermediate of composite insecticide chlorpyrifos.With trichloroacetic chloride and acrylonitrile as raw material and o-dichlorobenzene as solvent,3,5,6-trichloropyridin-2-ol sodium was synthesized by cyclization and aromatization on the catalyst of cuprous chloride and copper.The selection of solvent,the way of charging acrylonitrile,the reflux method,the reuse of catalyst and the repeated use of raw materials were investigated.When o-dichlorobenzene was used as solvent,acrylonitrile was added all at once and the reflux liquid went back below the liquid level,the catalyst could be used repeatedly for ten times,and the raw materials were reusable after distillation,which made the operation more convenient for industrial production.The total yield reached 84.1%.

关 键 词：三氯乙酰氯 丙烯腈 加成环化 芳构化 

分 类 号：TQ453.2[化学工程—农药化工]