Abstract: In accordance with the process of this invention, an improved catalyst for molecular oxidation of a hydrocarbon to form the corresponding carboxylic anhydrides is prepared by the steps of (a) forming a catalyst precursor by depositing on titanium dioxide solids in the anatase form at least a monolayer amount of at least one vanadium oxide source which is convertible to vanadium oxide upon calcining; (b) calcining the thus-formed catalyst precursor under conditions sufficient to convert the tantalum oxide source into the oxide form; (c) depositing upon the calcined catalyst precursor a catalytically effective amount of at least one vanadium oxide source which is convertible into vanadium oxide upon heating and at least one metal oxide source selected from the group consisting of oxides of Sb, Ga, Ge, In, T.sub.1, Pb, Se, Te, P and Bi, which is convertible into the corresponding metal oxide upon heating and which is reactive with V.sub.2 O.sub.