Abstarct: 4-nitro-phenylurazole was reacted with 2-bromoethanol, 1,2-dibromoethane and ethylchloroacetate in DMF as solvent, at mild to room temperature to produce 1,2-bis(2hydroxyethyl)-4-(4-nitrophenyl)-1,2,4-triazolidine-3,5-dione, 1,2-bis(2-bromoethyl)-4(4-nitropheny)-1,2,4-triazolidine-3,5-dione, and 1,2-bis(1-ethoxycarbonylmethyl)-4-(4nitropheny)-1,2,4-triazolidine-3,5-dione, respectively. The structure of the products were characterized by IR and 1H-NMR spectra. The reaction of 1,2-bis(2hydroxyethyl)-4-(4-nitropheny)-1,2,4-triazolidine-3,5-dione with equal moles of various diisocyanates, hexamethylene diisocyanate (HMDI), tolylene diisocyanate (TDI), and isophorane diisocyanate (IPDI), led to new polyurethanes, with good yields and inherent viscosities. The structure of these polyurethanes were confirmed using infrared spectroscopy, viscometery and thermal gravimetric analysis (TGA/DTG).