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Spent coffee grounds (SCGs) generated in coffee processing for beverages and other products are a very significant organic residue that needs to be properly treated. Waste valorization via oil extraction has the potential to obtain compounds that can be used for producing biodiesel or other high-value products, such as polymers. This work focuses on the ultrasound-assisted extraction of SCG oil using n-hexane as a solvent. Three key process parameters are analyzed: temperature, extraction time, and liquid/solid (L/S) rate of solvent, using a central composite rotatable design (CCRD), an analysis that, to the author’s knowledge, is not yet available in the literature. The data were analyzed using the software StatSoft STATISTICA 13.1 (TIBCO Software Inc., Palo Alto, CA, USA). Results show that all parameters have a statistical influence on the process performance (p < 0.05), being the L/S ratio the most significant, followed by extraction time and temperature. An analysis of variance (ANOVA) showed that the empirical model is a good fit to the experimental data at a 95% confidence level. For the range of conditions considered in this work, the optimal operating conditions for obtaining an oil extraction yield in the range of 12 to 13%wt are a solvent L/S ratio of around 16 mL g−1, for a temperature in the range of 50 to 60 °C, and the longest contact time, limited by the process economics and health and safety issues and also, by the n-hexane boiling temperature.