A new nanostructure poly(amide-imide) (PAI) was prepared from the polymerization of 4,4 0 -methylenebis(3-chloro-2,6-diethyl trimellitimidobenzene) as a diacid with 3,5-diamino-N-(4-hydroxyphenyl)-benzamide using triphenyl phosphite as a condensing agent and tetra-n-butylammonium bromide as a green media. The synthesized polymer was used to prepare PAI/ZnO nanocomposites (PZNC)s using nano-ZnO surface-coupled by N-trimellitylimido-L-alanine diacid as a coupling agent through ultrasonic process. The resulting PZNCs were also characterized by FT-IR, powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The TEM and FE-SEM results showed a good dispersion of nanoscale inorganic particles in the polymer matrix.