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  

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

作　　者：吕宝兰[1] 叶明琰[1] 徐玉林[1] 杨水金[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：《辽东学院学报（自然科学版）》2015年第1期1-6,共6页Journal of Eastern Liaoning University:Natural Science Edition

基　　金：湖北省自然科学基金重点项目(2014CFA131)

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H3PW12O40/Ti O2-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,H3PW12O40/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）=1.0∶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75min。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 H3PW12O40/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 H3PW12O40/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 tool, 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 rain. The yield of 3, 4 - dihydropyrimidine-2 （1H） -one derivatives could reach 53.7% -94.3%. The catalyst and synthesis prod- ucts were characterized by IR, XRD, SEM, respectively.

关 键 词：3 4-二氢嘧啶-2(1H)-酮衍生物 催化 H3PW12O40/TiO2-SiO2 

分 类 号：TQ426.91[化学工程]