In this study, the production of fatty acid ethyl esters (FAEE) from macauba pulp oil and pressurized ethanol was investigated. The experiments were conducted without the addition of catalyst, at 20 MPa, to determine the effect of temperature (200 to 300 °C) and the oil to ethanol mass ratio (1:1 and 1:2) on the FAEE content and different residence times (10 to 45 min). The effect of the addition of n-hexane to the oil (20 wt%) as a co-solvent was also evaluated. The use of high temperatures (275 and 300 °C) resulted in high FAEE content (∼90%). Increasing the amount of ethanol in the reaction medium contributed to the formation of esters only at operating temperatures of 200 to 250 °C. It was also observed that with the addition of co-solvent (in the oil) it was possible to obtain high amounts of FAEE in a shorter reaction time. In addition, a low content of unreacted compounds (∼8.0%) and the conversion of ∼90 and 99% of the free fatty acids and triglycerides were observed, respectively.