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Cocoa pod husk (CPH) is a potential material to produce value-added products. The objective of this study was to optimize the microwave-assisted hydrothermal pretreatment (MA-HTP) of CPH and CPH hemicellulose (HMC-CPH) using only water as the extraction medium, in combination with response surface analysis (RSA), Box–Behnken design (BBD), and proton nuclear magnetic resonance identification and quantification (¹H NMR Qu) to provide an efficient protocol for the extraction of mono- and disaccharides, as a novel method for which no precedent was found. The methodology consisted of 15 CPH MA-HTPs and 15 HMC-CPH MA-HTPs (triplicate) designed by RSA-BBD; the experimental variables were time, temperature, and power, and the response was the concentration of extraction products. Glucose, sucrose, and fructose were identified as products of the extractions by ¹H NMR. With 95% confidence, higher sucrose content was determined for CPH (45.62%) compared to HMC-CPH (17.34%), high fructose content for both CPH and HMC-CPH (37.88% and 35.37%, respectively), and minimal glucose concentrations were obtained in both CPH and HMC-CPH (4.57% and 0.93%, respectively). Using RSA-BBD, optimal temperature, power, and time points were predicted for glucose CPH: 135.4 °C, 180.6 W, and 5.8 min; sucrose: 154.3 °C, 256.3 W, and 20. 2 min; fructose 129.5 °C, 173.8 W, and 5.27 min. For HMC-CPH, the optimal conditions were as follows: glucose: 142.2 °C, 204.4 W, and 10.5 min; sucrose: 148.8 °C, 215.6 W, and 14.3 min; fructose: 151.6 °C, 231.6 W, and 13 min. Full article