壳聚糖钯催化Heck反应合成肉桂酸丁酯的研究  

Study on Heck Reaction for the Synthesis of Butyl Acrylate Catalyzed by Chitosan-supported Palladium

作　　者：刘蒲[1] 王岚[1] 刘一真[1] 

机构地区：[1]郑州大学化学系,河南郑州450052

出　　处：《分子催化》2004年第4期275-280,共6页Journal of Molecular Catalysis(China)

基　　金：2001年度河南省高校青年骨干教师资助计划.

摘　　要：以天然高分子壳聚糖为载体,制得了用于Heck反应的壳聚糖钯配合物多相催化剂,用XPS对其结构进行了表征,并利用正交实验方法考察了原料配比、缚酸剂三乙胺的用量、反应温度、反应时间和催化剂的用量对碘代苯与丙烯酸丁酯Heck反应的影响.结果表明:反应因素的影响大小为:反应温度>原料配比>三乙胺用量>催化剂的用量>反应时间;在最佳的反应条件下:碘代苯与丙烯酸丁酯的摩尔比为1∶1、三乙胺9mmol、催化剂0.1g(钯含量1.88×10-2mmol)时,氮气保护下140℃反应8h,肉桂酸丁酯的产率可高达99.8%.并且该催化剂对其它丙烯酸酯的Heck反应也具有良好的催化活性.A green heterogeneous catalyst for Heck reaction-chitosan-supported palladium complex was prepared, and its structure was characterized by XPS. Effects of the molar ratio of BA / PhI, Et3N / PhI, reaction temperature, reaction time and the amount of catalyst used on the yield were investigated by using orthogonal designation method. The sequence of the effect of the above factors is: reaction temperature > the molar ratio of BA / PhI > the molar ratio of Et3N / PhI > the amount of catalyst > reaction time. Under the optimal reaction conditions: 5 mmol PhI, 1∶1 molar ratio of PhI and butyl acrylate, 9 mmol Et3N, 0.1 g catalyst, 3 mL DMF, 140 ℃ for 8 hours, 99.8% yield of butyl cinnamate can be achieved. The catalyst also exhibits high activity and stereoselectivity to other acrylate and iodonitrobenzene.

关 键 词：壳聚糖 钯配合物 XPS 丙烯酸酯 HECK反应 正交实验设计 

分 类 号：O643.32[理学—物理化学]