氮配位的无磷聚合物负载钯配合物对Suzuki反应的催化性能

制备了结构简单、氮配位的无磷钯配合物聚氯乙烯-二乙烯三胺钯, 利用XPS, TG, DTA和TEM等手段对其进行了表征. 热分析表明PVC-DETA-Pd在室温至220 ℃范围内有很好的热稳定性; TEM分析证实, 钯在PVC-DETA-Pd中分布比较均匀, 钯颗粒呈球形, 粒径在15 nm左右, 并测定了在不同温度、时间、溶剂和底物等条件下对Suzuki反应的催化性能及重复使用性能. 结果表明, 在没有惰性气体保护的情况下, 以NaHCO₃作碱, 以DMF水溶液(体积比为2∶1)作溶剂, 在90 ℃时, 该配合物不仅对活性较高的碘代苯能够定量地催化, 对未活化的溴代苯也能定量地催化, 并且催化剂能够回收再利用8次以上.

Catalytic Property of Nitrogen-donor Phosphine-free Pd Complex Supported by Polymer in Suzuki Reaction

Nitrogen-donor polyvinyl chloride diethylene triamine palladium complex (PVC-DETA-Pd), the structure of which is simple and does not contain phosphine, was prepared, and the complex was characterized by XPS, TG, DTA, TEM, etc. Such PVC-DETA-Pd has good thermal stability from room temperature to 220 ℃. TEM confirmed that Pd particles are spherical and have uniform distribution with the size of about 15 nm. Then the catalytic property of the complex in Suzuki reaction and the property of recycle and reuse were determined under different temperature, time, solvent and the substrates. The results show that in the presence of NaHCO₃ as base and DMF-H₂O (volume ratio 2∶1) as solvent, the complex could catalyze not only iodobenzene but also non-activated bromobenzene quantitatively at 90 ℃ without the inert gas protection, and furthermore the catalyst could be recovered and reused more than eight times.