Department of Chemistry, GC University Lahore 54000, PakistanReceived September 6, 2012, Accepted September 13, 2012Presented study describes the synthesis of photo cross-linkable and water soluble hydroxyethyl starch hydroxy-ethyl methacrylate (HESHEMA) samples with different degree of substitution (DS) by functionalization ofhydroxyethyl starch (HES) with hydroxyethyl methacrylate (HEMA) or hydroxyethyl methacrylate carbonyl-imidazole (HEMACI) in DMSO using two different routes. It was revealed that the reaction time forHESHEMA synthesis can be reduced from 5 days to 24 h by conducting the reaction at 80