MCM-41固载胺钯配合物的制备及对Heck反应催化性能的研究有机化学.pdfVIP

2008 年第 28 卷 有 机 化 学 Vol. 28, 2008 第 5 期, 825～831 Chinese Journal of Organic Chemistry No. 5, 825～831 ·研究论文· MCM-41 固载胺钯配合物的制备及对 Heck 反应催化性能的研究 周健民*,a 杨育林 a 赵 岚 a 李校堃 周仁贤 b 郑小明 b a ( 温州医学院药学院 温州 325035) (b 浙江大学催化研究所 杭州 310028) 摘要 以 MCM-41 分子筛作为固载材料, 经氨基功能化后与各种钯化合物形成一系列 MCM-41 载钯配合物, 采用 XRD, XPS 等技术对其结构及表面性能进行了表征, 研究了催化剂的制备条件等因素对催化 Heck 芳基化反应性能的影 响; 以共轭烯烃和各种芳基碘的Heck 芳基化反应考察了 MCM～NH2•Pd(0, II)配合物的催化性能. 结果表明, MCM-41 的结构没有被破坏, MCM～NH2 载钯配合物具有较高的催化活性和立体选择性, 在较低的温度(70～90 ℃)下, 可高产 率地生成一系列取代的反式产物. 关键词 MCM-41; 钯配合物; 多相催化剂; Heck 反应 Synthesis of MCM-41 Supported Amino-palladium Complex and Its Catalytic Performance for Heck Reaction ZHOU, Jian-Min*,a YANG, Yu-Lina ZHAO, Lana LI, Xiao-Kuna ZHOU, Ren-Xianb ZHENG, Xiao-Mingb (a School of Pharmacy, Wenzhou Medical College, Wenzhou 325035) (b Institute of Catalysis , Zhejiang University, Hangzhou 310028) Abstract Using MCM-41 as supporter, a series of MCM-41 supported amino-palladium complexes have been prepared and characterized by XRD, XPS, etc. The XRD and XPS results indicate that the Pd coordi- nates with the NH2 groups on the MCM-41 surface, and the structure of MCM-41 has been not damaged. Its catalytic performance for Heck arylation of alkene with aryl iodide shows that the catalyst has high activity and stereoselectivity in 70～90 ℃. The product of Heck reaction takes E form. And the effect of the prepa- ration