Drying is an important step in the postharvest processing of agricultural products, as it allows the product to be preserved by reducing water activity to safe values, which stops microorganism growth and enzymatic reactions. In this context, the objective of this study was to assess how various drying temperatures, combined with ultrasonic pretreatment, affect drying rates and essential oil production. Assays were conducted according to a Central Composite Rotational Design, considering two factors with the following intervals: duration of the ultrasonic bath from 0 to 40 min, drying air temperature from 40 to 70 °C. The optimization was carried out using Response Surface Methodology (RSM). The essential oil was extracted by hydrodistillation and its constituents were identified by gas chromatography coupled to mass spectrometry. Histochemical analyses of fresh tubers were performed. The Midilli model was the one that best described the drying kinetics of Cyperus rotundus in all treatments. The drying time of C. rotundus tubers was dependent only on temperature (decreasing linear effect), it was possible to describe the variation in drying time as a function of temperature. It was not possible to adjust a model for ultrasonic bath time or drying temperature that would optimize both essential oil yield and the drying time of C. rotundus tubers. However, in this study, shorter drying times were observed compared to previous studies on C. rotundus tubers drying in the shade at room temperature. A total of 29 chemical constituents have been identified in the essential oil extracted from C. rotundus tubers, of which the majority are: 3,4-dimethyl-3-cyclohexen-1-carboxaldehyde (19.23%); caryophyllene oxide (17.63%); and α-cyperone (9.54%). Histochemical analyses of C. rotundus tubers showed the presence of starch, phenolic compounds, and lipids.