Abstract <p>Selective oxidation of alcohols to aldehydes is a crucial reaction for the preparation of valuable fine chemicals and bioactive compounds. Although various oxidants and methods exist, electrochemical oxidation stands out for its ability to efficiently synthesize aldehydes in high yields using simple salts as mediators. However, homogeneous catalysis often suffers from low yields, poor selectivity, and excessive oxidation to acids, which reduces its efficiency. In the present work, two-phase electrolysis has been successfully applied to the oxidation of benzyl alcohols―cinnamyl alcohol, 1-phenylethanol, 1-phenyl-1-propanol, and 2-phenylethanol―to their corresponding carbonyl compounds. The reaction was performed at ambient temperature in a beaker cell with C/SS electrodes, using CHCl₃ and aqueous NaCl (30%) with a catalytic amount of H₂SO₄ as the supporting electrolyte. The two-phase electrolysis achieved good to excellent aldehyde yields (52–71%) with a faradaic efficiency of 2F. This work demonstrates the potential of electrochemical oxidation as an efficient and selective method for aldehyde synthesis, offering a promising alternative to conventional approaches.</p>