We report the successful application of a templating approach employing ordered mesoporous carbon to the synthesis of BiVO4, Bi2Mo3O12, and Bi0.85V0.55Mo0.45O4 and the performance of these materials as catalysts for the oxidation of propene to acrolein. Ordered mesoporous carbon templates were used to control the nucleation and growth of the mixed metal oxide crystals, allowing higher final surface areas to be obtained. The resulting materials were characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and BET surface area analysis. The surface area of the mixed metal oxide catalysts was found to depend on the type of mesoporous silica used to prepare the carbon template and on the conditions under which the carbon template was formed. Through an appropriate choice of template, the surface areas of the mixed metal oxides exceeded 15 m(2)/g. Catalytic testing revealed that materials produced via templating in ordered mesoporous carbon had per-gram activities that were up to 85 times higher than those produced by a conventional hydrothermal synthesis and exhibited stable catalytic activities over 24 h.