6-氨基-4-苯基-2-碳硫双键-1,2-二氢嘧啶-5-甲酰胺的合成条件优化

Synthesis of 6-amino-4-phenyl-2-sulfanylidene-1,2-dihydropyrimidine-5-carboxamide compounds

以氰基乙酰胺、硫脲、苯甲醛为原料,一锅煮法合成6-氨基-4-苯基-2-碳硫双键-1,2-二氢嘧啶-5-甲酰胺,并对反应温度、反应时间、原料的投料比、反应介质以及对收率影响进行考察,产物经核磁进行表征。结果:在催化剂四水乙酸镍催化下,以氰基乙酰胺、硫脲、苯甲醛为原料发生"一锅煮"的3组分反应得到目标物,在氮气保护下并确定反应温度在70℃下回流反应7h,以1.0∶1.2∶1.5mmol投料比在THF中进行反应。本方法简单、产率高,节约时间和环境友好。

The process of preparing 6-amino-4-phenyl-2-sulfanylidene-1,2-dihydropyrimi-dine-5-carboxamide was investigated.Synthesis via one-pot reaction of cyanoacetamide、thiourea 、benzaldehyde using tetrahydrated nickel acetate as catalyst.The effect of reaction conditions on the yield was then inquired.The optimal reaction process were as follows：reaction with a nitrogen inletat 70 ℃ for 7 h,the raw ratio was 1.0：1.2：1.5,tetrahydrated nickel acetate as catalyst.this is a simple 、highly-yielding、time-saving and environmentally friendly method.