Mella Claudio, Torres Cecilia C, Pecchi Gina, Campos Cristian H
Depto. Físico-Química, Facultad de Ciencias Químicas, Universidad de Concepción, Edmundo Larenas 129, Concepción 4070371, Chile.
Depto. de Ciencias Químicas, Facultad de Ciencias Exactas, Universidad Andrés Bello, Sede Concepción, Autopista Concepción-Talcahuano 7100, Talcahuano 4300866, Chile.
Materials (Basel). 2019 Aug 16;12(16):2612. doi: 10.3390/ma12162612.
Palladium N,N'-bis(3-allylsalicylidene)o-phenylenediamine complex (PdAS) immobilized onto mesoporous polymeric methyl acrylate (MA) based resins (PdAS(x)-MA, x = 1, 2, 5, or 10 wt.%) were successfully prepared as heterogeneous catalysts for the Heck reaction. The catalysts were synthesized via radical suspension polymerization using PdAS as a metal chelate monomer, divinylbenzene and MA as co-monomers. The effect of the PdAS(x) content on the physicochemical properties of the resins is also reported. The catalysts were characterized by using a range of analytical techniques. The large surface area (>580 m·g) and thermal stability (up to 250 °C) of the PdAS(x)-MA materials allows their application as catalysts in the C-C coupling reaction between iodobenzene and MA in the presence of trimethylamine at 120 °C using DMF as the solvent. The PdAS(10)-MA catalyst exhibited the highest catalytic performance with no significant catalytic loss being observed after five reuses, thereby indicating excellent catalyst stability in the reaction medium.
成功制备了负载于介孔聚丙烯酸甲酯（MA）基树脂（PdAS(x)-MA，x = 1、2、5或10 wt.%）上的钯N,N'-双(3-烯丙基水杨醛)邻苯二胺配合物（PdAS），作为Heck反应的多相催化剂。通过自由基悬浮聚合，以PdAS作为金属螯合单体、二乙烯基苯和MA作为共聚单体合成了这些催化剂。还报道了PdAS(x)含量对树脂物理化学性质的影响。使用一系列分析技术对催化剂进行了表征。PdAS(x)-MA材料的大表面积（>580 m·g）和热稳定性（高达250°C）使其能够在120°C、以DMF为溶剂、三甲胺存在的条件下，作为碘苯与MA之间C-C偶联反应的催化剂。PdAS(10)-MA催化剂表现出最高的催化性能，在五次重复使用后未观察到明显的催化活性损失，从而表明该催化剂在反应介质中具有优异的稳定性。
