H_3PW_(12)O_(40)/SiO_2高效催化Mannich反应合成β-氨基酮衍生物  

Efficient one-pot synthesis of β-amino ketone derivatives catalyzed by H_3PW_(12)O_(40)/SiO_2

作　　者：陈慧媛[1] 徐玉林[1] 叶华林[1] 杨水金[1] 

机构地区：[1]湖北师范学院化学化工学院稀有金属化学湖北省协同创新中心(湖北师范学院),湖北黄石435002

出　　处：《湖北大学学报（自然科学版）》2015年第5期492-497,共6页Journal of Hubei University：Natural Science

基　　金：2013年国家级大学生创新创业训练计划项目(201313256001);湖北师范学院本科生科研项目(2014ZD31)资助

摘　　要：在室温条件下,采用浸渍法合成的H3PW12O40/Si O2为催化剂,高效催化酮、芳香醛和苯胺的Mannich反应合成系列β-氨基酮衍生物.对新型催化剂H3PW12O40/Si O2的制备条件进行优化,系统地研究了H3PW12O40负载量、焙烧温度、活化时间对催化剂的影响.探讨了H3PW12O40/Si O2对酮、芳香醛和苯胺的Mannich反应的催化活性,系统地研究了反应温度、催化剂用量、反应物的摩尔比等因素对产物收率的影响.实验结果表明：在n（酮）∶n（芳香醛）∶n（苯胺）=1.5∶1.2∶1.0,催化剂的用量占反应物料总质量的8%,反应温度为20℃,反应时间为9 h的最佳条件下,β-氨基酮衍生物的收率在61.2%-77.0%之间.整个反应体系具有条件温和、操作简单、不污染环境和催化剂可重复回收利用等优点.A new environmental friendly catalyst,H3PW12O40/Si O2 was prepared by impregnation method.The catalyst exhibited excellent catalytic activities for the synthesisis of β- amino ketone derivatives viaMannich reaction of ketones,aromatic aldehydes and aromatic amines. The preparation conditions of thecatalyst were conducted a comprehensive optimization. The effects of reaction on the yield of β-amino ketonewere investigated and the optimum conditions were determined as follows： n（ketones）∶n（aromatic aldehydes）∶n（aromatic amines）=1.5∶1.2∶1.0,the mass ratio of the catalyst to total reactant was 8%,the reaction temperaturewas 20 ℃,and the reaction time was 9 h. The yield of the product was up to 61.2% 77.0%. The results showthat the reaction catalyzed by H3PW12O40/Si O2 has advantages of mild reaction conditions,simple operation,easyisolation and the catalyst can be recycled.

关 键 词：H3PW12O40/SiO2 MANNICH反应 β-氨基酮 催化 

分 类 号：TQ426.91[化学工程]