Free radical homopolymerization of 2, -chloro 4 –nitro (phenyl) maleimide (N-CNPMI) was performed at 70 oC using Dimethylformamide (DMF) as a solvent and Benzoyl peroxide (BPO) as a free radical initiator to obtain homopolymer (H- DCPNPMI). The effect of different free radical initiators, solvents and time has been investigated. H-CNPMI is characterized by nitrogen percentage, FT-IR and 1H NMR analysis. Thermogravimetric analysis (TGA) characterizes the thermal stability of H-CNPMI. The initial decomposition temperature of HCNPMI was 180 oC. The gel permeation chromatography (GPC) determines the molecular weight (1198) and polydispersity index (PDI) 1.181 for H-CNPMI