Four supported Wacker-type catalysts were prepared by varying impregnation solvents and sequences of activated carbon. The catalysts were characterized by BET, XRD, SEM/EDXS, and TPR. They were tested for the dimethyl carbonate (DMC) synthesis from vapor-phase oxidative carbonylation of methanol. The results show that the preparation procedures have an impact on the reducibility, surface morphology as well as on the spatial distribution of the active-phase particles at the exterior of the carbon grains. Concerning the activity, the catalyst prepared by impregnating the carbon support with KOAc followed by PdCl2/CuCl2 employing ethanol as the impregnation solvent shows a higher performance in the oxidative carbonylation of methanol. The improved performance of the catalyst for methanol conversion to DMC can be attributed to the presence of a high surface concentration of an active phase comprising Pd and Cu species in close vicinity deposited on the external part of the carbon support. (C) 2004 Elsevier B.V. All rights reserved.