Hydroxyisoflavonoids were synthesized by an acylation-cyclization 2-step sequence.Reactions between the hydroxyisoflavonoids and perfluoroalkylsulfonyl fluorides produced 6 novel isoflavones containing perfluoroalkylsufonyl group.The perfluoroalkylsulfonylation of isoflavones containing 2 or 3 hydroxy groups showed high regioselectivity,namely only the 4′-hydroxy group in the isoflavones reacted with perfluoroalkylsulfonyl fluorides to give the corresponding perfluoroalkylsulfonylisoflavones,the structures of which were characterized by 1 HNMR,13C NMR,MS and IR spectra.