Pt-MoO x deposits synthesized by an electrochemical method are shown to be instable in methanol solutions at potentials ≥0.3 V. It is assumed that molybdenum oxides in the deposit composition react with methanol. The reduction of molybdenum compounds with methanol to form soluble Mo(+3) complexes in the presence of platinum is confirmed by spectrophotometric data. The MoO x reaction with methanol leads to the removal of molybdenum compounds from the electrode surface, which is accompanied by the loss of its catalytic activity in the methanol oxidation reaction.