Abstract
Condensation of 3-aminopropyltrimethoxysilane and chlorodiphenylphosphine in the molar ratio of 1:1 and 1:2 in the presence of Et3N in toluene afforded aminophosphine (CH3O)3Si(CH2)3NHPPh2 (L1) and bisphosphinoamine (CH3O)3Si(CH2)3N(PPh2)2 (L2) with methoxysilyl groups, respectively. Treatment of [(η6-C6H6)RuCl2]2 with L1 in refluxing tetrahydrofuran gave a mononuclear ruthenium phosphine complex [(η6-C6H6)RuCl2(κ1-P-L1)] (1). Reaction of [(η6-p-cymene)RuCl2]2 with L2 under the similar condition gave a dinuclear ruthenium phosphine complex [(η6-p-cymene)Ru(μ-Cl)3RuCl(κ2-P,P-L2)] (2). Complexes 1 and 2 were characterized by microanalyses, IR and NMR spectroscopies, and their structures were also established by single-crystal X-ray diffraction. Immobilization of complexes 1 and 2 on SBA-15, and characterization of these hybrid heterogeneous catalysts were studied by transmission electron microscopy (TEM), IR and low pressure N2 adsorption/desorption measurement. The heterogeneous catalysts were also briefly tested for transfer hydrogenation of acetophenone.
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