Heteropolycompounds, where one molybdenum atom of molybdophosphoric acid (M12P) was substituted by one vanadium atom, H4PMo11VO40, were synthesized and doped with Cu2+ or Fe3+. The prepared molybdovanadophosphates were characterized by Fourier transform infrared spectroscopy, P-31 nuclear magnetic resonance, diffuse reflectance spectroscopy, X-ray diffraction, thermal analysis, potentiometric titration, and cyclic voltammetry. The catalytic performance testing showed that the prepared materials have high catalytic activity for the room temperature conversion of 2,6-dimethylphenol to 2,6-dimethyl-1,4-benzoquinone using aqueous hydrogen peroxide as oxidizing agent. (C) 2007 Elsevier B.V. All rights reserved.