Soluble conjugated aromatic poly(1,3-dialkoxybenzene)s were obtained in high yield up to 80% in 30 min by grinding 1,3-dialkoxybenzene with anhydrous FeCl3 powder in a mortar at ambient and solvent-free condition. The polymers were characterized by FT-IR, H-1-NMR, C-13-NMR, and gel permeation chromatography. The structure of the aromatic rings linkage at meta-position was confirmed. Thermogravimetric analysis, UV-Vis, fluorescence spectroscopy, and four-probe a. c. technique were used to probe the thermal, optical, and electrical properties of the polymers. The polymers displayed high thermostability with the decomposition temperatures at about 382-388 degrees C. The optical energy gap (E-g) of the polymers was 4.23 eV and electrical conductivity at room temperature was 10(-6) S cm(-1). The fluorescence curve of the polymers displayed the maximum at 344 nm in CH2Cl2 solution. The morphology of the polymers was determined by X-ray diffraction and scanning electron microscope technique.