H_6P_2Mo_9W_9O_(62)/Zn(BDC)(Bipy)_(0.5)复合材料催化合成3,4-二氢嘧啶-2(H)酮衍生物  

Synthesis of 3,4-Dihydropyrimidine-2(H)-one Derivatives with H_6P_2Mo_9W_9O_(62)/Zn(BDC)(Bipy)_(0.5) as Catalyst

作　　者：向诗银 杨水金 XIANG Shi-yin YANG Shui-jin(College of Chemistry and Chemical Engineering, Hubei Normal University, Huangshi 435002, Chin)

机构地区：[1]湖北师范大学化学化工学院,湖北黄石435002

出　　处：《化学试剂》2017年第10期1039-1043,共5页Chemical Reagents

基　　金：湖北省自然科学基金重点项目(2014CFA131);2016年湖北省大学生创新创业训练计划项目(201610513010);湖北师范大学研究生创新基金项目(20160107)

摘　　要：采用水热法分别合成杂多酸H_6P_2Mo_9W_9O_(62)及有机金属骨架Zn(BDC)(Bipy)_(0.5),使用浸渍法合成H_6P_2Mo_9W_9O_(62)/Zn(BDC)(Bipy)_(0.5)复合材料,用该复合材料催化醛、乙酰乙酸乙酯和尿素通过Biginelli反应,乙醇作溶剂,合成6种3,4-二氢嘧啶-2(H)酮衍生物。通过IR、1HNMR、13CNMR确定其结构,通过m.p.确定其纯度。实验结果表明:固定醛用量为0.04 mol,n(醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.4∶1.5,2.0 wt%H_6P_2Mo_9W_9O_(62)/Zn(BDC)(Bipy)_(0.5),反应温度为105℃,反应时间为60 min时,产物收率为40.1%~91.5%。Six kinds of 3,4-dihydropyrimidine-2（H）-one derivative were prepared via Biginelli-typecondensation with ethyl acetoacetate,aromatic aldehyde and urea as starting materials,anhydrous ethanol as solvent and H6P2Mo9W9O62/Zn（BDC）（Bipy）0.5as catalyst.H6P2Mo9W9O62/ and Zn（BDC）（Bipy）0. 5was prepared by hydrothermal method,the catalyst was prepared by loading of heteropoly acid on metal organic skeleton by impregnation method.The structure was confirmed by IR,1HNMR,13 CNMR and it＇s purity was determined by melting point.The results showed that under the conditions of fixed aromatic aldehyde feed of 0. 04 mol,n（aromatic aldehyde） ∶ n（ethyl acetoacetate） ∶ n（urea） = 1 ∶ 1. 4 ∶ 1. 5,2. 0 wt% H6P2Mo9W9O62/Zn（BDC）（Bipy）0.5reaction temperature at 105 ℃ and reaction time of 60 min.The yield of the target products achieves 40. 1% ~ 91. 5%.

关 键 词：H6P2Mo9W9O62/Zn(BDC)(Bipy)0.5 Biginelli反应 3 4-二氢嘧啶-2(H)酮衍生物 

分 类 号：TQ460[化学工程—制药化工]