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无配体Pd/LDH-F催化剂在Heck和Suzuki反应中的应用

Application of Ligand-Free Pd/LDH-F Catalyst in Heck and Suzuki Coupling Reactions

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【作者】 周浩卓广澜姜玄珍张波葛忠华

【Author】 ZHOU Hao~1,ZHUO Guanglan~2,JIANG Xuanzhen~(1*),ZHANG Bo~3,GE Zhonghua~3(1 Department of Chemistry,Zhejiang University,Hangzhou 310027,Zhejiang,China;2 Department of Applied Chemistry,Zhejiang Sci-Tech University,Hangzhou 310012,Zhejiang,China;3 Department of Chemical Engineering,Zhejiang University of Technology,Hangzhou 310014,Zhejiang,China)

【机构】 浙江大学化学系浙江理工大学应用化学系浙江工业大学化工学院浙江工业大学化工学院 浙江杭州310027浙江杭州310012浙江杭州310027浙江杭州310014

【摘要】 以氟离子插层的水滑石LDH-F为载体,用逐滴浸渍法制备了新型Pd/LDH-F催化剂,并用其催化溴代芳烃的Heck和Suzuki偶联反应.用X射线衍射表征了催化剂的晶相,以等离子体发射光谱测定了溶剂中钯的流失量.结果表明,对于Heck反应,在无配体存在和低钯用量(Pd/溴代芳烃摩尔比为0.001)的情况下,Pd/LDH-F的催化性能优于其它载体负载的Pd催化剂,显示出很高的催化活性和选择性.在140℃和12 h的条件下,Pd/LDH-F催化溴苯与苯乙烯Heck反应产物的收率可达86%,反应后催化剂经过分离,可循环使用四次其催化活性基本不变.在DMF/水摩尔比为0.5的混合溶剂中,在室温和3h的条件下,Pd/LDH-F(Pd/溴代芳烃摩尔比为0.005)催化溴苯与苯基硼酸盐的Suzuki反应中,目标产物收率为99%.

【Abstract】 The palladium catalyst supported on fluoride pillared layered double hydroxide(LDH-F) was prepared by the incipient wetness method,and it was used to catalyze the Heck and Suzuki coupling reactions of aryl bromides.The structure of the Pd/LDH-F catalyst and the leaching of Pd in the solution were characterized by(X-ray) diffraction and inductively coupled plasma.With a small palladium dosage(Pd/aryl bromide molar ratio of 0.001) and no ligand,Pd/LDH-F exhibits higher catalytic activity and selectivity than the catalysts supported on other carriers for the Heck reaction of aryl bromides with styrene.The Pd/LDH-F catalyst can be easily separated from the reaction mixture and reused four times without loss in activity.Under the conditions of Pd/aryl bromide molar ratio of 0.005,room temperature and 3 h,the Pd/LDH-F catalyst can catalyze the Suzuki reaction of bromobenzene with a product yield of 99%.

【基金】 国家自然科学基金(20476092);绿色化学国家重点实验室资助项目
  • 【文献出处】 催化学报 ,Chinese Journal of Catalysis , 编辑部邮箱 ,2006年04期
  • 【分类号】O643.32
  • 【被引频次】19
  • 【下载频次】627
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