A new facile and rapid polycondensation reaction of 4,4'-(hexafluoroisopropylidene)-N,N'-bis(phthaloyl-L-leucine) diacid chloride (1) with several aromatic diols such as phenol phthalein (2a), bis phenol-A (2b), 4,4'-hydroquinone (2c), 1,4-dihydroxyanthraquinone (2d), 1,8-dihydroxyanthraquinone (2e), 1,5-dihydroxy naphthalene (2f), dihydroxy biphenyl (2g), and 2,4-dihydroxyacetophenone (2h) was performed by using 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 with the conventional solution polycondensation, and was completed within 10 min, producing a series of optically active poly(ester-imide)s with quantitative yield and high inherent viscosity of 0.50-1.12 dL/g. All of the above polymers were fully characterized by IR, elemental analyses, and specific rotation. Some structural characterization and physical properties of this optically active poly(ester-imide)s are reported.