无溶剂条件下一锅法合成3,4-二氢嘧啶-2(1H)-酮的研究  

One-pot synthesis of 3,4-dihydropyrimidin-2(1H)-ones under solvent-free conditions

作　　者：耿静漪[1] 张颖[1] 姜文清[1] 贾定先[1] 

机构地区：[1]苏州大学材料与化学化工学部,江苏苏州215123

出　　处：《化学研究与应用》2013年第12期1702-1706,共5页Chemical Research and Application

基　　金：国家自然科学基金项目(21171123)资助

摘　　要：无溶剂下,在无水硫酸氢钠催化作用下,由芳香醛、乙酰乙酸乙酯和尿素(或硫脲)三组分的Biginelli反应一锅法合成了一系列的3,4-二氢嘧啶-2(1H)-酮衍生物。通过四因素四水平的正交实验得到了优化的实验条件,利用薄板层析(TLC)确定了反应时间,同时考察了其他催化剂对Biginelli反应的影响。该方法具有反应条件温和、操作和后处理简单、产率高、污染少等特点。产物结构经IR、1H NMR分析确认。A series of 3,4-dihydropyrimidin-2-（1H）-one derivatives were synthesized by one-pot throe-component Biginelli reaction of aromatic aldehydes, ethyl acetoaeetate and urea or thiourea catalyzed by anhydrous NaHSO4 under solvent-froe conditions. The optimum reaction conditions were found out through an orthogonal test with four factors and four levels. Reaction time was confirmed u- sing thin layer chromatography（ TLC）, catalysts were also studied. The method had the advantages of mild reaction condition, simple operation and easy work-up, good yields and less pollution. The structures of final products were characterized by FT-IR and 1H NMR.

关 键 词：3 4-二氢嘧啶 2(1H)一酮 BIGINELLI反应 一锅法 无溶剂 无水硫酸氢钠 

分 类 号：TQ463.5[化学工程—制药化工]