The direct oxidation of p-methoxytoluene in acetic acid medium was studied on a graphite anode for the preparation of p-anisaldehyde and p-anisyl acetate. The effect of the water contents of the solvent on the reaction selectivity was determined for solvent mixtures containing from 0 to 20 vol % water. In anhydrous medium p-anisyl acetate was the main product. When the water contents increased the yield of p-anisaldehyde increased. It was shown that the higher the proportion of water, the lower the p-methoxytoluene oxidation rate. The formation of products of consecutive oxidation steps decreased as the temperature increased from 60 to 90 °C.