One-pot synthesis of metal primary phosphine complexes from O=PCl2R or PCl2R. Isolation and characterization of primary alkylphosphine complexes of a metalloporphyrin.
Treatment of [Ru(II)(Por)(CO)] [Por = porphyrinato(2-)] and O=PCl(2)R [R = Ad (adamantyl), Bu(t), Bu(sec)] or PCl2Mes (Mes = mesityl) with LiAlH4 afforded primary alkyl- and arylphosphine complexes [Ru(II)(Por)(PH2R)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)(PH2Ad)2] and [Ru(II)(F20-TPP)(PH2Mes)2] were determined by X-ray crystallography.
Huang
Jie-Sheng
JS
Department of Chemistry and Open Laboratory of Chemical Biology, Institute of Molecular Technology for Drug Discovery and Synthesis, University of Hong Kong, Pokfulam Road, Hong Kong. jshuang@hku.hk
Yu
Guang-Ao
GA
Xie
Jin
J
Zhu
Nianyong
N
Che
Chi-Ming
CM
D002713:Chlorine / Q000737:chemistry; D003460:Crystallization; D018360:Crystallography, X-Ray; D008024:Ligands; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D008665:Metalloporphyrins / Q000737:chemistry*; D008670:Metals / Q000737:chemistry; D008956:Models, Chemical; D008958:Models, Molecular; D010100:Oxygen / Q000737:chemistry*; D010720:Phosphines / Q000138:chemical synthesis* / Q000737:chemistry; D011522:Protons; D013055:Spectrophotometry, Infrared / Q000379:methods; D013056:Spectrophotometry, Ultraviolet
D008024:Ligands; D008665:Metalloporphyrins; D008670:Metals; D010720:Phosphines; D011522:Protons; D002713:Chlorine; D010100:Oxygen