新型杀菌剂氟吡菌酰胺的合成
Synthetic Process of Novel Fungicides Fluopyram
刘安昌 1冯佳丽 1贺晓璐 1张树康 1余彩虹1
作者信息
- 1. 武汉工程大学化学与环境工程学院,武汉430074
- 折叠
摘要
[目的]改进杀菌剂氟吡菌酰胺的合成工艺,提高总收率.[方法]以2,3-二氯-5-三氟甲基吡啶为原料,在碱的存在下与氰基乙酸乙酯经缩合,水解得到2-乙腈基-3-氯-5-三氟甲基吡啶;然后在钯碳催化下加氢得到2-乙胺基-3-氯-5-三氟甲基吡啶;在K2CO3为缚酸剂的作用下,2-乙胺基-3-氯-5-三氟甲基吡啶与邻三氟甲基苯甲酰氯反应得到目的产物氟吡菌酰胺.总收率44％.[结果]经1H NMR光谱鉴定,产品结构与氟吡菌酰胺结构一致.[结论]该工艺简单经济,条件温和,适合工业化生产.
Abstract
[Aims] The paper aims toimprove synthetic process and to increase yield.[Methods] 3-Chloro-5-(trifluoromethyl)-2-(2-aminoethyl)pyridine are prepared in high yield and selectivity by the cyanomethylation of 2,3-dichloro-5-(trifluoromethyl)pyridine with Et cyanoacetateto give a 3-chloro-5-(trifluoromethyl)-2-(2-cyanomethyl)pyridine which is then decarboxylated and catalytically hydrogenated by palladium (5％ on charcoal) into the 3-chloro-5-(trifluoromethyl)-2-(2-acetylaminoethyl)pyridine which is then subjected to HCl hydrolysis in water at reflux temperature.In the presence of K2CO3,3-chloro-5-(trifluoromethyl)-2-(2-aminoethyl)pyridineis reacted with 2-trifluoromethyl benzoic acid chloride to give the target compound fluopyam.The overall yield is above 44％ based on 2,3-dichloro-5-(trifluoromethyl) pyridine.[Results] The product thus obtained is identified with 1H NMR.[Conclusions] This process is simple,warm and economical,which is suitable for industrial scale manufacture.
关键词
杀菌剂/氟吡菌酰胺/合成Key words
fungicides/fluopyram/synthesis引用本文复制引用
出版年
2015
NETL
NSTL
维普
万方数据