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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%。
The heteropoly acid H_6P_2Mo_9W_9O_ (62) and the organometallic Zn (BDC) (Bipy) _ (0.5) were respectively synthesized by hydrothermal method. The H_6P_2Mo_9W_9O_ (62) / Zn (BDc) Materials, using the composite material catalyzed aldehyde, ethyl acetoacetate and urea by Biginelli reaction, ethanol as a solvent, synthesis of 6 3,4-dihydropyrimidine -2 (H) ketone derivatives. Its structure was confirmed by IR, 1HNMR, 13CNMR, and its purity was confirmed by m.p. The experimental results showed that the amount of aldehyde immobilized was 0.04 mol and the molar ratio of n (aldehyde): n (ethyl acetoacetate): n (urea) was 1: 1.4:1.5 and 2.0 wt% H_6P_2Mo_9W_9O_ (62) / Zn _ (0.5), the reaction temperature is 105 ℃, the reaction time is 60 min, the yield of product is 40.1% ~ 91.5%.