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Bis-aldehyde monomers 4-(4&#8242;-formyl-phenoxy)benzaldehyde (<b>3a</b>), 3-methoxy-4-(4&#8242;-formyl-phenoxy)benzaldehyde (<b>3b</b>), and 3-ethoxy-4-(4&#8242;-formyl-phenoxy)benzaldehyde (<b>3c</b>) were synthesized by etherification of 4-fluorobenzaldehyde (<b>1</b>) with 4-hydroxybenzaldehyde (<b>2a</b>), 3-methoxy-4-hydroxybenzaldehyde (<b>2b</b>), and 3-ethoxy-4-hydroxybenzaldehyde (<b>2c</b>), respectively. Each monomer was polymerized with <i>p</i>-phenylenediamine and 4,4&#8242;-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of <b>3b</b> and <b>3c</b> were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV&#8722;vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 &#215; 10^&#8722;5 to 6.4 &#215; 10^&#8722;5 Scm^&#8722;1, which was significantly higher than the values reported so far.