Triphenylphosphine oxide, OP(C6H5)3, can be conveniently prepared by oxidation of triphenylphosphine, P(C6H5)3, by oxygen under the catalytic effect of iron compounds such as FeX3 FeX3[OP(C6H5)3]2, (X = Cl, Br, NCS), or FeCl3[P(C6H5)32]. The highest catalytic effect was observed in the case of the complexes containing the bromo or thiocyanato ligands. The oxidation in acetonitrile solution is quantitative and selective at 30 - 70 °C and atmospheric pressure of oxygen gas.