The gas phase catalytic alkylation of phenol with methanol over new Sn-Ce-Rh-O catalyst has been studied. Cerium dioxide, tin dioxide, Sn-Ce-O and Sn-Rh-O systems have been also applied as catalysts. The reaction was carried out in a continuous process at the atmospheric pressure in dependence on temperature-starting at 523 K up to the deflection of phenol conversion. According to the elaborated method ortho-methyl phenol derivatives can be efficiently obtained. The best results were received in the presence of Sn-Ce-Rh-O: a summarized selectivity to ortho-cresol and 2,6-xylenol at 643 K reached 93.5% at the 71% conversion of phenol. Over all the studied catalysts O-alkylation was an insignificant process. (C) 2003 Elsevier Science B.V. All rights reserved.