Annually, millions of tons of foods are generated with the purpose to feed the growing world population. One particular eatable is orange, the production of which in 2018 was 75.54 Mt. One way to valorize the orange residue is to produce bioethanol by fermenting the reducing sugars generated from orange peel. Hence, the objective of the present work was to determine the experimental conditions to obtain the maximum yield of reducing sugars from orange peel using a diluted acid hydrolysis process. A proximate and chemical analysis of the orange peel were conducted. For the hydrolysis, two factorial designs were prepared to measure the glucose and fructose concentration with the 3,5-DNS acid method and UV-Visible spectroscopy. The factors were acid concentration, temperature and hydrolysis time. After the hydrolysis, the orange peel samples were subjected to an elemental SEM-EDS analysis. The results for the orange peel were 73.530% of moisture, 99.261% of volatiles, 0.052% of ash, 0.687% of fixed carbon, 19.801% of lignin, 69.096% of cellulose and 9.015% of hemicellulose. The highest concentration of glucose and fructose were 24.585 and 9.709 g/L, respectively. The results highlight that sugar production is increased by decreasing the acid concentration.