啶虫脒中间体N-(6-氯-3-吡啶甲基)甲胺合成工艺优化
发布时间:2019-08-14 13:55:43
发布时间:2019-08-14 13:55:43
啶虫脒中间体N-(6-氯-3-吡啶甲基)甲胺合成工艺优化
作者:王奇 侯申础 杨凡 王鑫 施武
来源:《中国化工贸易·中旬刊》2019年第01期
摘要:对N-(6-氯-3-吡啶甲基)甲胺的合成工艺进行优化。以2-氯-5-氯甲基吡啶、一甲胺为原料,在TEBAC的作用下合成N-(6-氯-3-吡啶甲基)甲胺。考察投料比、反应温度、滴加时间、溶剂等因素對N-(6-氯-3-吡啶甲基)甲胺收率的影响;研究发现,最佳反应条件为2-氯-5-氯甲基吡啶:一甲胺:TEBAC=1:7:0.012,滴加温度20-30°C,滴加时间2h,保温温度20-30°C,反应时间4hr,产品纯度可达96%,产品收率可达85-87%。
关键词:杀虫剂;N-(6-氯-3-吡啶甲基)甲胺;工艺优化
An Optimization of synthesis process of N-(6-chloro-3-pyridylmethylmethylamine)
(Jiangsu Yangnong Chemical Group Co., Ltd,Jiangsu Yangzhou 225009)
Abstract:The synthesis process of N-(6-chloro-3-pyridylmethylmethylamine) was optimized. N-(6-chloro-3- pyridylmethylmethylamine) was synthesized from 2-chloro-5-chloromethylpyridine and monomethylamine under the action of TEBAC. The effects of feed ratio, reaction temperature, dripping time and solvent on the yield of N-(6-chloro-3-pyridylmethylmethylamine) were investigated. The results showed that the optimum reaction conditions were 2-chloro-5-chloromethylpyridine: monomethylamine: TEBAC = 1:7:0.012, dripping temperature 20-30 °C , dripping time 2 h, holding temperature 20-30 °C , and reaction time 4 hr. The purity and yield of the product can reach 96% and 85-87%.