第 38 卷第 5 期Vol. 38 No. 5
2008 年 10 月Oct 2008

所属栏目:农药及中间体

一锅法合成2,3-二氯吡啶
冯 忖1,2,李 惠2,3,毛春晖2,杨 彬2,陈 明2 (1. 华中师范大学 化学学院,湖北 武汉 430079;2. 湖南化工研究院 国家农药创制工程技术研究中心,湖南 长沙 410007;3. 湖南师范大学 化学化工学院,湖南 长沙 410081)
摘 要:2,3-二氯吡啶是新型杀虫剂氯虫苯甲酰胺的关键中间体。比较了2,3-二氯吡啶的各种合成方法,探索了一条以3-氨基吡啶为原料,经过氯化、重氮化和sandmeyer反应,中间体不分离,一锅法合成2,3-二氯吡啶的经济合理的路线,收率66.9%,含量98%以上。对反应的机理进行了探讨,对副产物进行了分离与表征。
关键词:2,3-二氯吡啶;氯虫苯甲酰胺;一锅法;合成机理
中图分类号:TQ253.2  文献标识码:A  文章编号:1009-9212(2008)05- 0019-03
One-pot Synthesis of 2,3-Dichloropyridine
FENG Cun1,2,LI Hui2,3,MAO Chun-hui2,YANG Bing2,CHEN Ming2 (1.Department of Chemistry,Central China Normal University,Wuhan 430079,China;2. Hunan Research Institute of Chemical Industry (Hunan Research Institute of Pesticide),Changsha 410007,China;3.College of Chemistry and Chemical Engineering Hunan Normal University,Changsha 410081,China)
Abstract:2,3-Dichloropyridine is a key intermediate of a new insecticide chlorantraniliprole. Several synthesis routes of 2,3-dichloropyridine were evaluated in this paper,and therefore an economic and reasonable one-pot synthesis of 2,3-dichloropyridine was explored through chlorination,diazotization and sandmeyer reaction starting with 3-aminopyridine yield and purity of the product was 66.9% and 98% respectively. In additions of the mechanisms of reactions were studied and the by-products were separated and characterized.
Key words:2,3-dichloropyridine;chlorantraniliprole;one-pot synthesis;mechanism of synthesis
作者简介:冯 忖(1983-),男,陕西延安人,硕士研究生,从事有机合成方面的研究。(E-mail:fengcun1983@163.com)
联 系 人:毛春晖(1966-),男,副研究员,博士,主要从事农药及其中间体合成工艺研究。(E-mail:chmaocn@yahoo.com.cn)
收稿日期:2008-09-20