The oxidation of Alanine by Pyridinium chlorochromate has been studied by spectrophotometrically in the presence of perchloric acid in DMF-H2O medium. The reaction is first order with respect to PCC and fractional order with respect to [H+] and Alanine. Michaelis-Menten type kinetics was observed with alanine. The reaction rates were studied at different temperatures [25, 30, 35, 40, 45, 50 °C] and the activation parameters were computed. The reaction rate increased with increasing volume percentage of DMF in reaction mixture, suggesting the involvement of an ion and neutral molecule in the rate-determining step. The main reaction product were identified as chromium(III) and acetaldehyde. A suitable mechanism for the reaction was postulated.