Electrochemical polymerization of 3-allylanisole (4AA). via constant potential electrolysis, has been investigated in acetonitrile using two different supporting electrolytes. Redox behavior of the monomer was also studied in the same solvent-electrolyte couples at room temperature. Electrochemical polymerization of the monomer yielded insoluble polymer films on the electrode surface, which bears a very low conductivity, together with the low molecular weight polymers in the bulk of the solution. The decrease in the monomer concentration, during the electrochemical polymerization. was monitored by taking the cyclic voltammogram of the electrolysis solution. The effect of temperature on the rate of electrochemical polymerization was: also studied. The polymers were characterized by taking the H-1-NMR and FTIR spectra. Molecular weight of the soluble polymer was determined by vapor pressure osmometry. Thermal analysis of the polymer film and soluble polymer were done by DSC. (C) 2001 Elsevier Science Ltd. All rights reserved.