超声法合成3，4-二氢嘧啶-2（1H）-酮衍生物

摘要

以取代芳醛（1a～1h），乙酰乙酸乙酯（2）和脲（3）为原料，MMT／CuCl2为催化剂，乙醇为溶剂，在超声条件下经Beginelli反应合成了8个3，4-二氢嘧啶-2（1H）-酮衍生物（4a～4h），其结构经1H NMR和IR确证。以4a为例，分别采用单因素法和正交实验法研究了催化剂、溶剂、反应温度、超声时间和物料比r[n（1a）∶n（2）∶n（3）]对4a产率的影响。结果表明：在最优反应条件（1a 2．4 mol， r＝1．2∶1．0∶1．0， MMT／CuCl220 mol％， EtOH 1 mL，于90℃超声15 min）下，4a产率88．4％。MMT／CuCl2循环使用3次，产率基本不变。%An ultrasound-assisted synthetic method of 3,4-dihydropyrimidin-2(1H) one derivatives was developed, using aromaticaldehyde(1a~1h), ethylacetoacetate(2) and urea(3) as material, MMT/CuCl2 as catalyst and EtOH as solvent.The structures were confirmed by 1 H NMR and IR.Effects of catalysts, solvents, reaction temperature, ultrasonic time and molar ratio{r[n(1a) ∶n(2) ∶n(3)]}on yield of 4a were investigaed by single factor experiment and orthogonal test, respectively.The re-sults indicated that yield of 4a was 88.4% under the optimized conditoins(1a 2.4 mol, r=1.2 ∶1.0 ∶1.0, MMT/CuCl2 20 mol%, EtOH 1 mL, reaction at 90℃for 15 min).The yield of 4a remain stable after MMT/CuCl2 recycling for three times.