双核Pd-NHC配合物的合成及其催化Heck偶联反应  

Synthesis of Binuclear Pd-NHC Complex and Catalysted for Heck Coupling Reaction

作　　者：马学林 韩利民[1] 张骁勇[2] 段丽萍[2] MA Xue-lin;HAN Li-min;ZHANG Xiao-yong;DUAN Li-ping(College of Chemical Engineering,Inner Mongolia University of Technology,Hohhot 010051,China;Key Laboratory of Materials and Physical Chemistry,Department of Chemistry,Baotou Normal College,Baotou 014030,China)

机构地区：[1]内蒙古工业大学化工学院,内蒙古呼和浩特010051 [2]包头师范学院化学学院材料物理与化学重点实验室,内蒙古包头014030

出　　处：《化学试剂》2018年第11期1032-1036,共5页Chemical Reagents

基　　金：内蒙古自治区自然科学基金项目(2016MS0521,2018BS02009)

摘　　要：以1,4-二溴甲基苯和1,2,4-1H-三氮唑合成N-取代苄基三氮唑盐,通过PdCl3、N-取代苄基三氮唑盐与吡啶耦合,合成了一种新型苄基型双核Pd-NHC催化剂。产物通过IR、1HNMR、13CNMR和元素分析等进行了表征。综合考察了催化剂对Heck偶联反应的催化性能。结果表明,这种新型苄基型双核Pd-NHC催化剂对Heck偶联反应表现出较高的催化产率和选择性。最佳工艺条件为：物质的量分数0. 5%的Pd-NHC为催化剂,4 mL DMF为溶剂,3 mmol K3PO4碱性介质,温度控制在100℃,反应时间为4 h,催化产率可达89%,顺反异构选择性可控制在17∶1。The N-substituted benzyl triazole salt was synthesized with 1,4-bis（ bromomethyl） benzene and 1,2,4-1 H-triazole. A new catalyst of N-Heterocyclic carbene（ NHC） binuclear Pd-complexes has been successfully prepared by Coupling-ligand with PdCl3,N-substituted benzyl triazole salt and pyridine in good yields.The products were characterized by means of IR,1 HNMR,13CNMR and elemental analysis.The catalyst was investigated comprehensively which was applied to Heck coupling reaction.The results show that the new Pd-NHC catalyst has higher catalytic yield and selectivity for Heck coupling reaction.The best process：0. 5% mass fraction of Pd-NHC catalyst,4 mL DMF,3 mmol K3 PO4,100 ℃,4 h,the catalytic yield is up to 89%,and the cis and trans isomerization can be controlled in 17 ∶1.

关 键 词：双核氮杂环卡宾 Pd-NHC催化剂 HECK偶联反应 

分 类 号：O621.2[理学—有机化学]