A series of poly(1,4-phenylene terephthalates) with pendant NLO chromophores was prepared by the solution polycondensation of 2,5-NLO chromophore substituted terephthalic acid with hydroquinone. The polymers obtained gave satisfactory NMR and elemental analysis results when taking into account their expected structures and the inherent viscosity value proved the polymeric character of all polymers. DSC, optical polarizing microscopy and WAXS studies revealed that none of these polymers exhibited liquid crystalline mesophases. Preliminary results on NLO properties of these polymers showed a surprisingly large second harmonic signal relative to a Y-cut quartz plate.