A new and efficient method for preparation of optically active poly (styrene-divinylbenzene) copolymers (PS-DVB) is presented here. This is carried out by Friedel-Crafts acylation reaction of chiral N-phthaloyl L-leucine acid chloride with PS-DVB beads in the presence of aluminum chloride as Lewis acid catalyst and 1,2-dichloroethane as the solvent at ambient temperature. Reagents' amounts and reaction conditions are mentioned and four samples with different amounts of functionality have been prepared. Final products were characterized by FT-IR and elemental analysis. The results obtained confirm that the above modification in preparation of chiral supported PS-DVB has been achieved well and in moderate yield. (C) 2002 Elsevier Science B.V. All rights reserved.