The preparation of new poly(urethaneimide)s (PUIs) having acceptable thermal stability and higher flame resistance was aimed. Two new aromatic diisocyanate-containing methyldiphenylphosphine oxide and triphenylphosphine oxide moieties were synthesized via Curtius rearrangement in situ and polymerized by various prepared diols. Four aliphatic hydroxy terminated aromatic based diols were synthesized by the reaction between ethylene carbonate and various diphenolic substances. Chemical structures of monomers and polymers were characterized by FTIR, 1 H NMR, 13 C NMR, and 31 P NMR spectroscopy. Thermal stabilities and decomposition behaviors of the PUIs were tested by DSC and TGA. Thermal measurements indicate that the polymers have high thermal stability and produce high char. Polymers exhibit quite high fire resistance, evaluated by fire test UL-94. The films of the polymers were prepared by casting the solution. Inherent viscosities, solubilities, and water absorbtion behaviors of the polymers were reported in. V

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The synthesis of N,N′‐bis(4′‐amino‐4‐biphenylene) isophthalamide (BABPI) and its applicability as a new diamine for the preparation of a series of new, high Tg, perfectly alternating poly(amide‐imide)s is described. BABPI was synthesized from the catalytic reduction of the corresponding dinitro compound which was prepared by the condensation of isophthaloyl chloride and 4‐amino‐4′‐nitrobiphenyl. The modified selective reduction technique was used for the preparation of 4‐amino‐4′‐nitrobiphenyl from 4,4′‐dinitro‐biphenyl. Poly(amide‐imide)s were synthesized by polycondensation of diamine BABPI with various commercially available aromatic dianhydrides via a conventional two‐step procedure. In the first step, poly(amic‐acid)s were prepared in a polar aprotic solvent, such as N‐methyl pyrrolidone (NMP) at room temperature. Depending on the dianhydride used, intrinsic viscosities of poly(amic‐acid)s were found to range between 0.43–0.69 dL/g. Bulk thermal imidization technique was used to obtain fully imidized poly(amide‐imide)s at the second step. The synthesized poly(amide‐imide)s showed good thermal stability up to 320°C and the 10% weight loss temperatures were recorded in the range of 525–550°C as evidenced by thermogravimetric analysis (TGA). The glass transition temperatures were found to be between 225–235°C from differential scanning calorimeter (DSC) measurements. © 1997 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 35: 1149–1155, 1997