Phosphine oxides receive less attention than phosphines mainly because of their appearance as byproducts (Wittig, Staudinger) or impurities. Our interest in different phosphine oxides is based on their potential to probe oxide surfaces. The focus of this presentation is threefold: (i)  Quick and selective methods for the oxidation of phosphines and (ii)  analytical differences between phosphine oxides and their H2O2 and H2O adducts are explored. (iii)  Methods for the safe and efficient purification of phosphine oxides are communicated. After H2O2 oxidation of phosphines, solid-state and solution 31P NMR, and IR spectroscopy reveal distinct features of the phosphine oxides and their H2O2 adducts. Furthermore, the X-ray structures of Bu3P=O and [Cy3P=O�(H2O2)]2 show different characteristics, with the adduct displaying an unprecedented cyclic structure incorporating six oxygen atoms (Dalton Trans., in press). A method for the quantitative decomposition of bound H2O2, and simultaneous removal of adsorbed H2O within 1h is presented.

Synthesis, purification, and characterization of phosphine oxides and their hydrogen peroxide adducts

243rd National Meeting (2012)

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