Various mixed oxides were tested as catalysts for oxidative dehydrogenation of hydroxyacetone to form pyruvaldehyde (2-oxopropanal). The best results were obtained from an iron phosphate with a P/Fe atomic ratio of 1.05. The yield of pyruvaldehyde reached 88%. The next best results were obtained from a supported heteropoly acid (H3PMo12O40) The other molybdenum- and vanadium-based oxide catalysts were not suitable. The effects of the composition and structure of iron phosphate and the effects of reaction variables on the formation of pyruvaldehyde were also studied.