Synthesis of dihydroxybisimide monomers and their subsequent polycondensation with dichlorophenylphosphine oxide by use of a phase-transfer catalyst are reported. The monomers were characterized by melting point, elemental analysis, and IR spectroscopy. The polyimidophosphonates were characterized by viscosity measurement, molecular weight determination, elemental analysis, IR, ESCA, H-1-NMR, P-31-NMR, and X-ray diffraction. Thermal stability and glass transition temperature (T,) of the polymers were evaluated by TGA, DTA, and TMA. These polymers are self-extinguishing and readily soluble in highly polar solvents like DMF, DMSO, DMAC, NMP, HMPA, etc.