A new facile and rapid polycondensation reaction of 4,4'-(hexafluoroisopropylidene)-N,N'-bis(phthaloyl-L-leucine) diacid chloride (1) with several aromatic diamines, including benzidine (2a), 4,4'-diaminodiphenyl methane (2b), 1,5-diaminoanthraquinone (2c), 4,4'-sulfonyldianiline (2d), 3,3'-diaminobenzophenone (2e), P-phenylenediamine (2f), 2,6-diaminopyridine (2g), 4,4' -diaminobenzophenone (2h), 2,4-diaminotoluene (2i), and 4,4'-diaminodiphenylether (2j), was developed with a domestic microwave oven in the presence of a small amount of a polar organic medium such as o-cresol. The polymerization reactions proceeded rapidly compared to conventional solution polycondensation and finished within 12 min, producing a series of optically active poly(amide-imide)s with quantitative yields and high inherent viscosities of 0.50-1.93 dL/g. All of the polymers were fully characterized by In, elemental analyses, and specific rotation. Some structural characterization and physical properties of these optically active poly(amide-imide)s are reported.