H_3PW_(12)O_(40)/TiO_2-SiO_2催化合成3,4-二氢嘧啶-2(1H)-酮衍生物  

Catalytic Synthesis of 3,4-Dihydropyrimidine-2(1H)-one Derivatives with H_3PW_(12)O_(40)/TiO_2-SiO_2

作　　者：杨水金[1] 蔡红莲[1] 徐玉林[1] 

机构地区：[1]湖北师范学院化学化工学院,湖北黄石435002

出　　处：《商丘师范学院学报》2014年第12期53-57,共5页Journal of Shangqiu Normal University

基　　金：湖北省自然科学基金重点项目(ZRZ2014000118)

摘　　要：以H3PW12O40/TiO2-SiO2为催化剂,取代苯甲醛、乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂合成3,4-二氢嘧啶-2(1H)-酮衍生物.探讨了原料物质的量比、反应温度、催化剂用量及反应时间对收率的影响.实验表明:固定取代苯甲醛的用量为0.04 mol和无水乙醇的量为15 m L的情况下,n(取代苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.0∶1.5,催化剂的用量占反应物料总质量的1.5%,反应温度为90℃,反应时间为75 min,分别以对羟基苯甲醛、对硝基苯甲醛、茴香醛、4-氯苯甲醛、对甲氧基苯甲醛分别代替苯甲醛,产品收率为35.0%-89.2%.催化剂和合成产品分别采用IR,XRD和1H NMR,IR,MS手段进行表征.3, 4 -Dihydropy -rimidine -2 （ 1H ） -one was synthesized from substituted benzaldehyde, ethylacetoacetate and urea using H3 PW12 O40/TiO2 -SiO2 as a novel eco-friendly catalyst that 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 for synthesis of 3,4-dihydropy-rimidine-2（1H） -one.When the dosage of substituted benzaldehyde is 0.04 mol, and anhydrous ethanol as solvent,n（substituted benzaldehyde）∶n（ethyl acetoacetate）∶n（urea） =1.0∶1.0∶1.5, the quantity of catalyst is 1.5%quantity of the feed stock, and reaction temperature is 90℃, and reaction time 75 min, the yield of 3,4-dihydropyrimidine-2（1H）-one could reach 35.0%-89.2%.The catalyst and synthesis products were characterized by IR, XRD and 1H NMR, IR, MS, respectively.

关 键 词：H3 PW12 O40/TiO2 -SiO2 3 4-二氢嘧啶酮 

分 类 号：TQ426.91[化学工程]