Abstract We herein report a simple, efficient, and high‐yielding oxidation method of aldehydes to carboxylic acids bearing functional groups. With operationally simple procedures and a wider scope of aliphatic and aromatic aldehydes, the developed protocol furnishes an excellent yield of carboxylic acid relevant to industrial and academic research. Advantageously, the developed protocol directly delivers ester derivative from aldehyde in the presence of alcohol with given conditions. The reaction proceeds via sulfate radical anion (SRA), and a plausible reaction mechanism is proposed accordingly.