A biphase electrolysis method has been developed for the preparation of aldehydes. Ceric ammonium sulphate (CAS) in aqueous acidic medium is an effective for the electro oxidation of alcohols in dichloromethane to the corresponding carbonyl compounds using graphite electrodes at room temperature. Electro oxidation resulted in high yield (83-99%) of aldehydes from primary alcohols than that of Ex-cell method and CAS was regenerated and reused for further reactions in biphasic electrolysis medium.