Production of polyol ester from esterification of hexanoic acid (HA) and neopentyl glycol (NPG) was investigated. An optimization experiment, using a Taguchi L9 experimental layout, was used to examine the effect of temperature, pressure, HA:NPG ratio and catalyst amount. The effects of pressure (0.5, 25 and 50 kPa); temperature (423, 453 and 483 K); catalyst amount (0.5, 1.0 and 1.5 w/w) and HA:NPG ratio (1.5:1, 3:1 and 6:1) were investigated and found to have impacts on the reaction. The percentage contribution of each factors are 43.9, 38.8, 4.3 and 12.9 , respectively. At the optimal reaction conditions of 423 K, 0.5 kPa, sulfuric acid catalyst 0.5 w/w and HA:NPG ratio (3:1) more than 99 w/w neopentyl glycol ester was obtained. Confirmation experiments were performed to demonstrate the effectiveness of this approach and characterization of neopentyl glycol ester was characterized using FTIR and 1H NMR.