摘要
4,5,6-三取代嘧啶类化合物是重要的医药中间体,对其合成工艺进行优化。以氰基乙酰胺、苯甲醛、尿素为原料,一锅煮法合成目标化合物,并对反应时间、反应温度、反应介质以及原料的投料比对收率的影响进行考察,产物经核磁进行表征。结果:在四水乙酸镍催化下,以氰基乙酰胺、苯甲醛、尿素为原料发生"一锅煮"的三组分反应得到4,5,6-三取代嘧啶,在氮气保护下并确定反应温度在70℃下氰基乙酰胺、苯甲醛、尿素以1.0:1.2:1.5毫摩尔比在THF中回流反应7小时。该方法简单、产率高,节约时间和环境友好。
The process of preparing 4, 5, 6 - trisubstituted pyrimidine Compounds, as one ot most important intermediate for synthesis was investigated. Synthesis via one -pot reaction of cyanoacetamide, benzaldehyde, urea or thiourea using nontoxic tetrahydrated nickel acetate as catalyst. The influence of reaction conditions on the yield was then inquired. The optimal reaction conditions were as follows： the raw ratio was 1.0： 1.2 ： 1.5, tetrahydrat- ed nickel acetate as catalyst, reaction with a nitrogen inletat 70℃ for 7h. The products were characterized with 1H -NMR. this is a simple, highly -yielding, time -saving and environmentally friendly method.
出处
《宜春学院学报》
2014年第3期9-11,共3页
Journal of Yichun University
基金
国家重大新药创制(2012ZX09303009_002)
安徽省教育厅高校省级自然科学项目(kj2013z055)
安徽科技学院青年基金(ZRC2013341)
关键词
4
5
6-三取代嘧啶
一锅法合成
TLC跟踪
氢谱
4, 5, 6 - trisubstituted Pyrimidine
One - pot Synthesis
TLC Tracking
1H - NMR
