In this project, a series of new optically active poly(ester-imide-imine)s (PEIIs) and poly(azo-ester-imide)s (PAEIs) based on L-leucine, L-isoleucine, L-alanine, and L-phenylalanine were synthesized and some physical properties of them were investigated.At first using above amino acids and pyromellitic dianhydride or 3,3´,4,4´-Benzenetetracarboxylic-3,3´,4,4´-dianhydride, optically active diacids N,N´ -pyromelliticdiimido-di-L-amino acids (1a-1d) and N,N´ -(3,3´,4,4´-Benzophenone tetracarboxylic)-3,3´,4,4´-diimido-di-L-amino acids (2a-2d) were synthesized in two steps and then chlorinated, using thionyl chloride as chlorinating agent. Other new monomers were 4-(4-((4-hydroxyphenylimino) methyl)benzylidene amino)phenol, from the reaction between terephthaldialdehyde and 4-amino phenol, and new colorful monomers 4,4´-sulfonyl bis (4,1-phenylene) bis (diazene-2,1-diyl) diphenol, 4,4´-oxi bis (4,1-phenylene) bis (diazene-2,1-diyl) diphenol 4,4´-methylene bis (4,1-phenylene) bis (diazene-2,1-diyl) diphenol, from diazo coupling reaction between 4,4´-diamino diphenyl sulfone, 4,4´-diamino diphenyl ether, 4,4´-diamino diphenyl methane, and phenol. The structure of the above monomers were fully characterized by elemental analysis, FT-IR and 1 H NMR spectroscopy. New optically active PEII s were synthesized via Interfacial polycondensation reaction. Inherent viscosities of these polymers were in the range of 0.13-1.25 dL g -1 and have good thermal stability. Then in the second project, these polymers again were synthesized, using microwave irradiation. Inherent viscosities were in the range of 0.09-0.13 dL g -1 . Comparing the two sets of results, and physical properties, it seems that interfacial polycondensation can result in polymers with higher yields, higher viscosities, more retention of optical activity of chiral monomers, and also better colors. In the third project, a series of new optically active PAEIs were synthesized via interfacial polycondensation reaction. Inherent viscosities were in the range of 0.32-0.57 dL g -1 ., and they have moderate thermal stability. All of the above polymers were characterized by FT-IR spectroscopy, and elemental analysis.