The photopolymerization of methyl methacrylate (MMA) through the use of diethyl dithiocarbarnato(1,2)-propane diol (DCPD) was studied. The photoinitiator was synthesized from 3-chloro-1,2-propane diol and sodium diethyl dithiocarbamate in a solvent mixture of acetone and anhydrous ethanol. The photopolymerization was carried out in a Heber multilamp photochemical reactor (COMPACT-LP-MP88) (Heber Scientific, Chennai, India) at 254 nm. The effects of the reaction conditions on the polymerization of MMA were studied. The conversion and molecular weight increased with an increase in the monomer concentration and reaction time. However, for the DCPD-to-MMA molar ratio, a critical value was found for maximum conversion. The results suggested the living radical nature of the photoinitiator, which was further investigated by the preparation of a block copolymer with styrene. (c) 2005 Wiley Periodicals, Inc.