A series of W-V-O catalysts with different m-WO 3 and h-WO 3 phase contents were hydrothermally synthesized by employing different tungsten, vanadium, and ammonium precursors and characterized by powder XRD, N 2 adsorption, SEM, X-ray energy-dispersive spectroscopy, thermogravimetric analysis, Raman and FTIR spectroscopy, NH 3 temperature programmed desorption, H 2 temperature-programmed reduction, and XPS. Finally, the acid/redox properties were analyzed by using aerobic transformation of methanol as a characterization reaction. A correlation between phase composition as well as acid and redox properties was observed, which were correlated to the catalytic performance of the title materials in a one-pot [a]