Polyester polyols were synthesized by using each one mole of sebacic acid, isophthalic acid, ethylene glycol, and neopentyl glycol. The synthesized polyol had 56.6 mg KOH/g of hydroxy value and 1980 g/mole of molecular weight. From FT-IR structure analysis of polyester polyol, Hydroxy group(-OH) was observed around 3600 cm(-1), - CH shoulder of sebacic acid at 2950 cm(-1), carbony group of ester around 1730 cm(-1), and benzene ring of isophthalic ring was represented at 1600 cm(-1), 740 cm(-1). In case of polyurethane, hydroxy peak was showed at 3600 cm(-1), and - NH group around 3300 cm(-1), 1530 cm(-1). From H-1 NMR measurement of polyester polyol, it was found that sebacic acid was represented at 1.3, 1.5, 2.1 ppm, isophthalic acid at 7.3, 8.1, 8.7 ppm, ethylene glycol at 4.2 ppm, and neopentyl glycol at 0.8, 3.2, 3.9 ppm, respectively. In the polyurethane, it is almost the same as spectrum of polyester polyol, but showed very week peak at 7 ppm by benzene ring of toluene diisocyanate.