催化学报 ›› 2006, Vol. 27 ›› Issue (4): 335-338.

• 研究论文 • 上一篇    下一篇

无配体Pd/LDH-F催化剂在Heck和Suzuki反应中的应用

周浩1,卓广澜2,姜玄珍1,张波3,葛忠华3   

  1. 1 浙江大学化学系, 浙江杭州 310027; 2 浙江理工大学应用化学系, 浙江杭州 310012; 3 浙江工业大学化工学院, 浙江杭州 310014
  • 收稿日期:2006-04-25 出版日期:2006-04-25 发布日期:1984-12-26

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

ZHOU Hao1, ZHUO Guanglan2, JIANG Xuanzhen1*, ZHANG Bo3, GE Zhonghua 3   

  1. 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
  • Received:2006-04-25 Online:2006-04-25 Published:1984-12-26

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3 h 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%.

关键词: 钯, 氟, 水滑石, 负载型催化剂, 溴代芳烃, Heck反应, Suzuki反应

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%.

Key words: palladium, fluoride, layered double hydroxide, supported catalyst, aryl bromide, Heck reaction, Suzuki reaction