Poly(1,3-dimethoxybenzene) was synthesized via the electrochemical oxidation of the corresponding monomer (1,3-dimethoxybenzene) in an acetonitrile solution containing tetrabutylammonium tetrafluoroborate (Bu 4 NBF 4 ) and characterized spectroscopically. The resulting polymer is insoluble in all common solvents. Structural characterization using Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR) spectroscopies suggests that this material has a polymeric structure in which the methoxy groups are retained. Spectroscopic results are in good agreement with theoretical calculations based on a proposed structure. Electrical conductivity at room temperature is 2.5 10 - 4 S cm - 1 .