One-pot synthesis of metal primary phosphine complexes from O=PCl 2R or PCl 2R. Isolation and characterization of primary alkylphosphine complexes of a metalloporphyrin

Abstract

Treatment of [Ru II(Por)(CO)] [Por = porphyrinato(2-)] and O=PCl 2R [R = Ad (adamantyl), Bu t, Bu sec] or PCl 2Mes (Mes = mesityl) with LiAlH 4 afforded primary alkyl- and arylphosphine complexes [Ru II(Por)(PH 2R) 2], which have been isolated in pure form and characterized by 1H NMR, 31P NMR, IR, and UV-vis spectroscopy and mass spectrometry. The structures of [Ru II(TTP)(PH 2Ad) 2] and [Ru II(F 20-TPP)(PH 2Mes) 2] were determined by X-ray crystallography. © 2006 American Chemical Society.