An efficient and convenient procedure for the synthesis of 2-perfluoroalkyl ethanoic acids by direct oxidation of 2-perfluoroalkyl ethanols with Jones' reagent (CrO 3H 2SO 4 is described. Treatment of the acids with aqueous sodium hydroxide gave 3-perfluoroalkyl, 3-fluoro-2, 3- propenyl carboxylic acids which may be used for the preparation of the corresponding chlorides and amides.