extraction of M. fistulifera seeds with hexane provided an oil rich in tryacylglycerides of linolenic and linoleic acids, presenting iodine index of 182.15 g of I2 per 100 g of oil. In this study, the synthesis of polyols from M. fistulifera oil using an in situ hydroxylation procedure is described. Univariate assays were applied to determine the optimal reaction time of 720 min. In addition, a 22 factorial central composite design was carried out containing 12 experimental assays that allowed the investigation of different molar ratios of the reagents used in polyol synthesis, as well as the applicability of polyols for the preparation of rigid polyurethanes.