偕胺肟纤维-钯(II)配合物催化溴吡啶与苯硼酸的偶联反应研究

Research on Catalyzed Bromopyridine Phenylboronic Coupling Reaction with [Pd(II)-AOFs]

摘要:

以偕胺肟化的聚丙烯腈纤维为配体，制备了偕胺肟纤维-钯(II)配合物[Pd(II)-AOFs]，考察了Pd(II)-AOFs催化溴吡啶与苯硼酸偶联反应活性。结果显示，Pd(II)-AOFs对溴吡啶与苯硼酸及其衍生物的偶联反应展现出良好的催化活性。工艺优化结果表明：Pd(II)-AOFs（0.6 mol%）、溴吡啶（5 mmol），苯硼酸（5.5 mmol）、NaHCO3（10 mmol）为碱试剂、乙醇:水（V/V=2:1） 30 ml为溶剂、回流条件下，反应产率可达到90%以上，且表现出很宽的底物适应性，重复使用7次后产率仍达到90%。向反应体系中加入四丁基溴化铵（10 mol%），可大为缩短反应时间。

Abstract:

The modified polyacrylonitrile fiber was used as carrier to prepare Pd(II)-AOFs. The catalytic performance of Bromopyridine and Phenylboronic acid coupling reaction on Pd(II)-AOFs was investigated. The results showed that the yield of [Pd(II)-AOFs] could reach 90% under following conditions: Bromopyridine (5 mmol), phenylboronic acid (5.5 mmol), solvent (C2H5OH/H2O, V/V=2:1, 30 ml), base (NaHCO3, 10 mmol), TBAB(10 mol%), reflux reaction time (30 min), Pd (II)-AOFs (0.6 mol%).The reaction also had a good adaptability on Bromopyridine and Phenylboronic acid/Its Derivatives coupling reaction, after repeated seven times the production was still 90%.When added TBAB the reaction time is greatly shorten.