Abstract [Hydroxy (sulfonyloxy) iodo] perfluoroalkanes (C n F 2n+ 1 I+ OH⊎− OSO 2 R, n= 3, 4, 6; R= p-CH 3 C 6 H 4, CF 3) can be prepared in two steps from the corresponding perfluoroalkyliodides by oxidation with pertrifluoroacetic acid and subsequent reaction with TsOH or Me 3 SiOTf. These compounds react with trimethylsilyl derivatives of aromatic compounds under mild conditions forming the corresponding perfluoroalkyl (aryl) ...