Several azo-monomers were prepared from the diazotation of m-phenylene diamine using different aromatic amines. Side chain azo-polyimides were prepared by the reaction of stoichiometric mole ratio of the prepared azo-monomers with four different dianhydride monomers to produce the corresponding polyamic acids then changed to the appropriate azo-polyimides by dehydration using acetic anhydride and pyridine in (4:1) ratio, then allowed to irradiate under microwave to ensure completely imidation. Structures of the prepared compounds were characterized using IR, H-NMR and 13C-NMR spectrometer and LC-Mass. In addition, solubility, inherent viscosity and thermal properties were studied for the prepared azo-polymers.