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乙二胺功能化树脂负载Pd(0)配合物:可重复使用的高活性Heck芳基化催化剂
引用本文:杨元法,庄明,曾朝霞,黄朝表,罗孟飞.乙二胺功能化树脂负载Pd(0)配合物:可重复使用的高活性Heck芳基化催化剂[J].中国化学,2006,24(10):1309-1314.
作者姓名:杨元法  庄明  曾朝霞  黄朝表  罗孟飞
作者单位:Institute of Physical Chemistry Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces,Zhejiang Normal University,Jinhua,Zhejiang 321004,China,Zhejiang Normal University,Jinhua,Zhejiang 321004,China,Institute of Physical Chemistry,Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces,Zhejiang Normal University,Jinhua,Zhejiang 321004,China,Zhejiang Normal University,Jinhua,Zhejiang 321004,China,Institute of Physical Chemistry,Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces,Zhejiang Normal University,Jinhua,Zhejiang 321004,China
摘    要:The ethylenediamine-functionalized resin-supported Pd(0)complex was prepared from PdCl_2 and ethylenedia-mine-functionalized chloromethylated polystyrene,followed by reduction with KBH_4.The complex was character-ized by FT-IR,XRD,BET,SEM and EDS.The resin-supported catalyst exhibited high catalytic activity in theHeck reaction and could be reused up to 17 times in NMP or 16 times in DMF at 90 ℃ in the Heck reaction of io-dobenzene with acrylic acid.The leaching investigation disclosed that the palladium leaching was caused by the in-teraction of iodobenzene with the metal Pd(0)on supported catalyst.The leached palladium species in filtrate wasvery stable and could be reused five times after the solid catalyst was filtered off.A cross-transfer test in recyclingin the presence of additional carbon disclosed that the soluble leached palladium species had much higher catalyticactivity than supported and/or adsorbed palladium in solid-solution heterogeneous Heck reaction.

关 键 词:Heck反应  再生  树脂支持钯(0)配合物  乙烯基二胺功能化树脂  浸取
收稿时间:2006-01-26
修稿时间:2006-01-262006-06-29

Ethylenediamine-Functionalized Resin-Supported Pd(0) Complex:An Effective and Recyclable Catalyst for Heck Vinylation
YANG Yuan-Fa, ZHUANG Ming, ZENG Chao-Xia, HUANG Chao-Biao, LUO Meng-Fei.Ethylenediamine-Functionalized Resin-Supported Pd(0) Complex:An Effective and Recyclable Catalyst for Heck Vinylation[J].Chinese Journal of Chemistry,2006,24(10):1309-1314.
Authors:YANG Yuan-Fa  ZHUANG Ming  ZENG Chao-Xia  HUANG Chao-Biao  LUO Meng-Fei
Institution:1. Institute of Physical Chemistry, Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Zhejiang Normal University, Jinhua, Zhejiang 321004, China; 2. Zhejiang Normal University, Jinhua, Zhejiang 321004, China
Abstract:The ethylenediamine‐functionalized resin‐supported Pd(0) complex was prepared from PdCl2 and ethylenediamine‐functionalized chloromethylated polystyrene, followed by reduction with KBH4. The complex was characterized by FT‐IR, XRD, BET, SEM and EDS. The resin‐supported catalyst exhibited high catalytic activity in the Heck reaction and could be reused up to 17 times in NMP or 16 times in DMF at 90 °C in the Heck reaction of iodobenzene with acrylic acid. The leaching investigation disclosed that the palladium leaching was caused by the interaction of iodobenzene with the metal Pd(0) on supported catalyst. The leached palladium species in filtrate was very stable and could be reused five times after the solid catalyst was filtered off. A cross‐transfer test in recycling in the presence of additional carbon disclosed that the soluble leached palladium species had much higher catalytic activity than supported and/or adsorbed palladium in solid‐solution heterogeneous Heck reaction.
Keywords:Heck reaction  recycling  resin-supported Pd(O)complex  ethylenediamine-functionalized resin  leaching
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