The synergy in CdMoO4/MoO3 catalysts has been investigated in selective oxidation of C4 hydrocarbons. Both of the pure phases, MoO3 and CdMoO4, as well as the two-phase catalyst have been characterized using X-ray diffraction, BET surface area measurement, scanning electron microscopy and laser Raman spectroscopy. Oxidation studies performed over the CdMoO4/MoO3 catalyst and its pure-phase constituents, using both 1-butene and 1,3-butadiene as feed material, show that the two-phase catalyst had a higher selectivity to maleic anhydride than either of the pure phases. This synergistic effect is similar to the one previously observed over MnMoO4/MoO3 catalysts. © 1990.