The kinetics of oxidation ofacidic α-amino acids, namely aspartic acid and glutamic acid using N-Iodosuccinimide (NIS), in acetic acid-water medium in the presence of hydrochloric acid at 303 K has been studied. The reaction shows inverse first order with respect to oxidant and [H+]. Increase in [amino acid] has a slight positive effect on the rate, indicating first order dependence. Addition of salts like K2SO4, Na2SO4, KCl to the reaction medium has no effect on the rate, Increase in temperature increases the rate of the reaction. The amino acids were oxidized to corresponding aldehydes, carbon dioxide, and ammonia. The products obtained were isolated and identified. The activation parameters have been computed. A mechanism confirming to the kinetic observations is suggested.