第 43 卷第 2 期Vol. 43 No. 2
2013 年 4 月Apr 2013

所属栏目:农药及中间体

4-氯-6-甲氧基嘧啶回收利用的工艺研究
彭志海1,2,3,刘卫东2,3,朱卫国1,杜升华2,3 (1. 湘潭大学 化学学院,湖南 湘潭 411105;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 410014;3. 农用化学品湖南省重点实验室,湖南 长沙 410014)
摘 要:4-氯-6-甲氧基嘧啶是杀菌剂嘧菌酯生产过程的主要副产物。本文研究了4-氯-6-甲氧基嘧啶与三光气反应得到4,6-二氯嘧啶的方法,可使4-氯-6-甲氧基嘧啶回收变为嘧菌酯生产的原料。确定了优化工艺条件为:8.8 g(0.06 mol)4-氯-6-甲氧基嘧啶(CMP)、13.2 g(0.18 mol)N,N-二甲基甲酰胺(DMF),n(BTC)∶n(CMP)=1∶1,100℃反应2 h,收率为93.2%,该方法具有操作简便,环境友好,产品收率和含量较高,适合工业化生产等优点。
关键词:嘧菌酯;4-氯-6-甲氧基嘧啶;4,6-二氯嘧啶
中图分类号:S482.2  文献标识码:A  文章编号:1009-9212(2013)02-0017-03
Study on the Recycling of 4-Chloro-6-methoxypyrimidine
PENG Zhi-hai1,2,3,LIU Wei-dong2,3*,ZHU Wei-guo1,DU Sheng-hua2,3 (1. College of Chemistry,Xiangtan University,Xiangtan 411105,China;2. National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry,Changsha 410014,China;3. Hunan Province Key Laboratory for Agrochemicals,Changsha 410014,China)
Abstract:4-Chloro-6-methoxypyrimidine (CMP)is a main by-product resulted in the production process of fungicide azoxystrobin. Recovery of CMP by reaction with bis(trichloromethyl)carbonate to the formation of 4,6-dichloropyrimidine was developed. The optimal reaction conditions were obtained with the molar ratio of CMP to DMF and BTC to CMP were 1 to 3 and 1 to 1,respectively,and rthe reaction was run at 100℃ for two hours. The process has various advantages,including easy operation,environmentally friendly,good yields and convenient for scaled production.
Key words:azoxystrobin;4-chloro-6-methoxypyrimidine;4,6-dichloropyrimidine
基金项目:2013年湖南省创新团队项目:绿色农药研究。
作者简介:彭志海(1988-),男,湖南娄底人,硕士研究生,研究方向为农药工艺研究。(E-mail:peng_zhi_hai200@163.com)
收稿日期:2013-04-05