Complex metal oxides of transition metals using Mo, W, V, Nb and Ta were synthesized by hydrothermal method. The synthesized complex metal oxides were characterized and the solid acid catalytic activity was tested through the Friedel-Crafts alkylation of anisole and benzyl alcohol. X-ray diffraction patterns of the obtained samples showed two peaks at 2 theta = 22 degrees and 46 degrees indicating these materials have layer-type crystal structure, regardless of the combination of several metals. Moreover, Mo-V-O, Mo-Nb-O, W-Nb-O and W-Ta-O showed microporosity from N-2 adsorption isotherm. Among of these combinations, Mo-Nb-O, W-Nb-O and W-Ta-O showed a higher catalytic performance for alkylation reaction. (C) 2011 Published by Elsevier B. V.