The electrochemical oxidation of p-xylene in a methanol solvent catalyzed by monometal and multimetal compounds to methoxyl p-xylene derivatives on a pair of porous graphite plane electrodes with a chemical conversion of > 80% was described and investigated. From the results of ultraviolet-visible (UV-Vis) spectroscopy, X-ray photoelectron spectroscopy (XPS), powder X-ray diffractometry (XRD), gas chromatography-mass spectrometry (GC-MS), and fluorescence spectroscopy, a possible free-radical reaction mechanism was proposed.