Abstract Perfluoroalkyl acetic acids, RF CH 2 COOH, can be prepared in several ways. Particular attention is here paid to the method starting from the azonitrile-initiated addition of the corresponding perfluoroalkyl iodide, RFI, to vinyl acetate, CH 2 CHOCOCH 3, with formation of the adduct RF CH 2 CHIOCOCH 3. This method is reported as a four-step process that synthesizes perfluoroalkyl acetic acids through the conversion of the adduct ...