芳香炔基共轭微孔聚合物固载有机钯金属催化剂的合成及其催化Suzuki偶联反应的效率探索

Synthesis of conjugated microrous polymers based on aromatic alkynyl skeleton immoblized palladium acetate and exploration of the efficiency of catalystic Suzuki couping reaction

以4,4'-二溴联苯和甲基丁炔醇为原料,成功合成了单体4,4'-二乙炔基联苯.通过4,4'-二乙炔基联苯和均三溴苯在不同反应浓度下的偶联聚合,分别成功制备了共轭微孔聚合物HCMP-C1和HCMP-C2,采用1H NMR、13C NMR、FI-IR等表征手段确认了单体和聚合物结构.将醋酸钯通过物理吸附负载于HCMP-C2上,成功制备出催化剂Pd@HCMP-C2.此催化剂的催化性能优异,实现了苯硼酸和对碘甲苯短时高效的Suzuki偶联反应,1.5 h转化率高达99%.

4,4'-dibromobiphenyl and methylbutynol were used as basic materials, synthesis of 4,4'-diethynylbiphenyl was achieved by coupling reaction, afterward HCMP1 and HCMP2 was obtained by a polymerization of 4,4'-diacetylenylbiphenyl and 1,3,5-tribromobenzene at different reaction concentrations. The structures of the monomers and polymers were confirmed by 1H-NMR, 13C-NMR and FI-IR analysis etc. Then palladium was physically loaded on the HCMP2 as Pd@HCMP-C2 catalyst. Pd@HCMP-C2 has showed excellent catalytic activity in Suzuki coupling reaction. Phenylboronic Acid and p-Iodotoluene can be efficiently converted into 4-Methylbiphenyl with the high yield of 99%, only 1.5 hours reaction time.