摘要
以偕胺肟化的聚丙烯腈纤维(AOFs)为载体和配体,与PdCl2溶液反应,制备偕胺肟-Pd(Ⅱ)配合物纤维[AOFs-Pd(Ⅱ)]。以苯硼酸与碘苯为反应体系,DMF/H2O(V/V=1)水相体系为溶剂,考察AOFs-Pd(Ⅱ)催化Suzuki反应的催化性能,并研究其催化机理。研究结果表明:AOFs-Pd(Ⅱ)对Suzuki反应具有很好的催化性能,能重复使用6次以上,且反应底物上取代基团的性质对AOFs-Pd(Ⅱ)催化性能没有影响。在1.34 g(11.0 mmol)苯硼酸、1.12 mL(10.0 mmol)碘苯、0.15 g AOFs-Pd(Ⅱ)、30 mL溶剂DMF/H2O(V/V=1)、2.77 g(33 mmol)NaHCO3,90℃下加热反应5 h,产率达95%以上;并提出了AOFs-Pd(Ⅱ)催化反应的机理。
Amidoxime fibers-palladium( Ⅱ ) complex (AOFs- Pd( Ⅱ ) ) was prepared by reaction of PdC12 with polyacrylo- nitrile fibers containing amidoxime groups, fibers were used as carrier and ligand. The catalytic performance and mechanism for Suzuki reactions of phenylboronic acid with iodobenzene were investigated in DMF and H20 mixture solvent( V/V = 1 ). The results show that AOFs-Pd( Ⅱ ) had a high catalytic activity for the reaction and can be used repeatedly over 6 times,and substituent groups of reaction substrate have no effect for its catalytic properties. When phenylboronic acid was 1.34 g ( 11.0 mmol) , aryl iodide was 1.12 mL ( 10. 0 mmol) ,AOFs-Pd( IⅡ ) was 0. 15 g,NaHCO3 was 2.77 g(33 mmol) ,DMF/H20( WV = 1 ) was 30 mL,reaction time was 5 h and reaction temperature was 90℃, the yield was more than 95%. The catalytic mechanism of AOFs-Pd ( Ⅱ ) was proposed.
出处
《化学试剂》
CAS
CSCD
北大核心
2012年第9期792-796,共5页
Chemical Reagents
基金
国家自然科学基金资助项目(21171003
20771002)