The title compounds are obtained by direct hydrolysis of the corresponding 2/4- perfluoroalkyl-substituted anilines and anisoles by the system AcOH/HBr/H2O/Al2O3. A two- step preparation of 2/4-perfluoroacylanilines involves the treatment of the 2/4- perfluoroalkylaniline with sodium ethoxide followed by hydrolysis of the resultant diethyl acetal with hydriodic acid.