A poly(imide benzoxazole) was prepared directly from trimellitic anhydride chloride and 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BisAPAF) monomers in a two-step method. In the first step, a poly(hydroxyamide amic acid) precursor was synthesized by the low-temperature solution polymerization in an organic solvent. Subsequently, thermal cyclodehydration of the poly(hydroxyamide amic acid) precursor at 350degreesC produced the corresponding poly(imide benzoxazole). The inherent viscosity of the precursor polymer was 0.22 dL/g. The cyclized poly(imide benzoxazole) showed a glass transition temperature (T-g) at 329degreesC and a 5% weight loss temperature at 530degreesC in nitrogen and at 525degreesC in air. The poly(imide benzoxazole) is amorphous as evidenced by the wide-angle X-ray diffraction measurement. The structures of the precursor polymer and the fully cyclized polymer were characterized by Fourier transform infrared (FTIR) and proton nuclear magnetic resonance spectroscopy (H-1 NMR). (C) 2003 Wiley Periodicals, Inc.