Buscemi Roberto, Giacalone Francesco, Orecchio Santino, Gruttadauria Michelangelo
Dipartimento di Scienze e Tecnologie Biologiche, Chimiche e Farmaceutiche (STEBICEF), Sezione di Chimica, Università di Palermo, Viale delle Scienze s/n, Ed. 17, 90128 Palermo (Italy), Fax: (+39) 091-596825.
Chempluschem. 2014 Mar;79(3):421-426. doi: 10.1002/cplu.201300361. Epub 2014 Jan 23.
Five imidazolium-based materials have been synthesised and used for the first time as palladium scavengers. Radical reactions of suitable bis-vinylimidazolium salts led to a series of insoluble materials through homo-polymerisation, immobilisation with a 3-mercaptopropyl-modified silica gel or co-polymerisation with ethylene glycol dimethylacrylate. These materials were screened as palladium scavengers with a set of palladium(0) and palladium(II) compounds in different solvents and at different starting amounts of palladium. In many cases, residual amounts of palladium were lower than 5 ppm, as requested for the manufacture of active pharmaceutical ingredients and fine chemicals. The application of one of these materials as a palladium scavenger in a Suzuki coupling reaction resulted in a 29-fold abatement of the palladium content in the final product with respect to the control reaction.
已合成了五种咪唑鎓基材料，并首次将其用作钯清除剂。合适的双乙烯基咪唑鎓盐的自由基反应通过均聚、与3-巯基丙基改性硅胶固定或与乙二醇二甲基丙烯酸酯共聚，生成了一系列不溶性材料。这些材料在不同溶剂中、不同钯起始量的情况下，用一组钯(0)和钯(II)化合物作为钯清除剂进行了筛选。在许多情况下，钯的残留量低于5 ppm，这是活性药物成分和精细化学品生产所要求的。其中一种材料作为钯清除剂应用于铃木偶联反应中，相对于对照反应，最终产物中的钯含量降低了29倍。
