The buriti palm (Mauritia flexuosa) is a palm tree widely distributed throughout tropical South America. The oil extracted from the fruits of this palm tree is rich in natural antioxidants. The by-products obtained from the buriti palm have social and economic importance as well, hence the interest in adding value to the residue left from refining this oil to obtain biofuel. The process of methyl esters production from the buriti oil soapstock was optimized considering acidulation and esterification. The effect of the molar ratio of sulfuric acid (H2SO4) to soapstock in the range from 0.6 to 1.0 and the reaction time (30–90 min) were analyzed. The best conditions for acidulation were molar ratio 0.8 and reaction time of 60 min. Next, the esterification of the fatty acids obtained was performed using methanol and H2SO4 as catalyst. The effects of the molar ratio (9:1–27:1), percentage of catalyst (2–6%) and reaction time (1–14 h) were investigated. The best reaction conditions were: 18:1 molar ratio, 4% catalyst and 14 h reaction time, which resulted in a yield of 92% and a conversion of 99.9%. All the key biodiesel physicochemical characterizations were within the parameters established by the Brazilian standard. The biodiesel obtained presented high ester content (96.6%) and oxidative stability (16.1 h).