Synthesis and characterization of water-soluble palladium(II)-functionalized diphosphine complexes
摘要:
Water-soluble functionalized bis(phosphine) ligands L (a-h) of the general formula CH2(CH2PR2)(2), where for a: R = (CH2)(6)OH; b-g: R = (CH2)(n)P(O)(OEt)(2), n = 2-6 and n = 8; h: R = (CH2)(3)NH2 (Scheme 1), have been prepared photochemically by hydrophosphination of the corresponding 1-alkenes with H2P(CH2)(3)PH2. Water-soluble palladium complexes cis-[Pd(L)(OAc)(2)] (1-8) were obtained by the reaction of Pd(OAc)(2) with the ligands a-h in a 1:1 mixture of dichloromethane: acetonitrile. The water-soluble phosphine ligands and their palladium complexes were characterized by IR, H-1 and P-31 NMR. A crystallographic study of complex 1 shows that the Pd(II) ion has a square planar coordination sphere in which the acetate ligands and the diphosphine ligand deviate by less than 0.12 angstrom from ideal planar. (C) 2009 Elsevier Ltd. All rights reserved.