H3PW12O40／TiO2－SiO2催化合成3，4－二氢嘧啶－2（1H）－酮衍生物

摘要

以取代苯甲醛，乙酰乙酸乙酯和尿素为原料，以溶胶凝胶法制备的H3 PW12 O40／TiO2－SiO2为催化剂，催化合成3，4－二氢嘧啶－2（1H）－酮衍生物，考察了三组分摩尔比、反应温度、催化剂用量、反应时间对反应收率的影响。研究表明， H3 PW12 O40／TiO2－SiO2是合成3，4－二氢嘧啶－2（1H）－酮衍生物的良好催化剂，在取代苯甲醛的用量为0．04 mol， n （取代苯甲醛）∶n （乙酰乙酸乙酯）∶n （尿素）＝10．∶1．2∶1．5，催化剂的用量占反应物料总质量的2．5％，反应温度为90℃，反应时间为75 min。在此优化条件下，3，4－二氢嘧啶－2（1H）－酮衍生物的收率可达53．7％～94．3％。催化剂经IR、XRD、 SEM表征。%The 3, 4 -Dihydropy -rimidine -2 (1H) -one derivatives was synthesized from substituted benzaldehyde, ethylacetoacetate and urea using H3 PW12 O40/TiO2 -SiO2 as a novel eco-friendly catalyst that was prepared by a sol-gel technique.The influences of molar ratio of reactant, reaction temperature, catalyst dosage and reaction time were discussed.Experimental results showed that H3 PW12 O40/TiO2 -SiO2 is a good catalyst to synthesize 3, 4-dihydropy-rimidine-2 (1H) -one derivatives.When the dosage of substituted benzaldehyde is 0.04 mol, n (substituted benzaldehyde) ∶n (ethylacetoacetate) ∶n (urea) =1.0∶1.2∶1.5, the quantity of catalyst is 2.5%of the feed stock, reaction temperature is 90℃and reaction time is 75 min.The yield of 3, 4-dihydropy-rimidine-2 (1H) -one derivatives could reach 53.7%~94.3%.The catalyst and synthesis prod-ucts were characterized by IR, XRD, SEM, respectively.