A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H ...A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.展开更多
目的合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮。方法采用一锅法Biginelli反应以乙酰乙酸乙酯、苯甲醛和尿素为原料,H3PW12O40/SiO2为催化剂,无水乙醇为溶剂进行合成目标化合物。通过熔点,IR,1 H NMR和MS等测试手段对合成的...目的合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮。方法采用一锅法Biginelli反应以乙酰乙酸乙酯、苯甲醛和尿素为原料,H3PW12O40/SiO2为催化剂,无水乙醇为溶剂进行合成目标化合物。通过熔点,IR,1 H NMR和MS等测试手段对合成的目标化合物进行表征。结果探讨了反应温度、催化剂用量、反应时间和反应物的摩尔比对收率的影响。实验表明:固定苯甲醛用量为0.04mol的条件下,催化剂的用量占反应物料总质量的2.0%,n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.5∶1.5,反应时间为90min,反应温度为90℃。在优化条件下,产品平均收率可达79.2%。结论溶胶凝胶法制备的H3PW12O40/SiO2是合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的良好催化剂,具有催化剂用量少,催化活性高,可回收重复使用等特点。展开更多
采用浸渍法制备H3PW12O40/TiO2-SiO2催化剂,以环己酮和乙二醇为原料合成环己酮乙二醇缩酮。实验考察了环己酮与乙二醇物质的量比、催化剂用量、反应时间对收率的影响。结果表明,H3PW12O40/TiO2-SiO2催化剂是合成环己酮乙二醇缩酮的良好...采用浸渍法制备H3PW12O40/TiO2-SiO2催化剂,以环己酮和乙二醇为原料合成环己酮乙二醇缩酮。实验考察了环己酮与乙二醇物质的量比、催化剂用量、反应时间对收率的影响。结果表明,H3PW12O40/TiO2-SiO2催化剂是合成环己酮乙二醇缩酮的良好催化剂,确定了最佳合成条件:n(环己酮)∶n(乙二醇)=1∶1.4,催化剂用量为反应物料总质量的0.8%,反应时间45 min,带水剂环己烷用量为6 m L;此条件下环己酮乙二醇缩酮收率可达77.6%。展开更多
文摘A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.
文摘目的合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮。方法采用一锅法Biginelli反应以乙酰乙酸乙酯、苯甲醛和尿素为原料,H3PW12O40/SiO2为催化剂,无水乙醇为溶剂进行合成目标化合物。通过熔点,IR,1 H NMR和MS等测试手段对合成的目标化合物进行表征。结果探讨了反应温度、催化剂用量、反应时间和反应物的摩尔比对收率的影响。实验表明:固定苯甲醛用量为0.04mol的条件下,催化剂的用量占反应物料总质量的2.0%,n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.5∶1.5,反应时间为90min,反应温度为90℃。在优化条件下,产品平均收率可达79.2%。结论溶胶凝胶法制备的H3PW12O40/SiO2是合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的良好催化剂,具有催化剂用量少,催化活性高,可回收重复使用等特点。
基金supported by the National Key Basic Research Program of China(973)(2010CB226903)National Natural Science Foundation of China(21073147,21303140)Program for Changjiang Scholars and Innovative Research Team in University,China(IRT1036)~~
文摘采用浸渍法制备H3PW12O40/TiO2-SiO2催化剂,以环己酮和乙二醇为原料合成环己酮乙二醇缩酮。实验考察了环己酮与乙二醇物质的量比、催化剂用量、反应时间对收率的影响。结果表明,H3PW12O40/TiO2-SiO2催化剂是合成环己酮乙二醇缩酮的良好催化剂,确定了最佳合成条件:n(环己酮)∶n(乙二醇)=1∶1.4,催化剂用量为反应物料总质量的0.8%,反应时间45 min,带水剂环己烷用量为6 m L;此条件下环己酮乙二醇缩酮收率可达77.6%。
