采用水热法分别合成杂多酸H6P2Mo9W9O62及有机金属骨架Zn(BDC)(Bipy)0.5,使用浸渍法合成H6P2Mo9W9O62/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%H6P2Mo9W9O62/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%.