Corn pericarp (CP) is an inexpensive agroindustrial by-product that is available in large quantity in Mexico. This work aimed to optimize the use of a dilute sulfuric acid pretreatment for CP hydrolysis to maximize the reducing sugars yield. A 2-step experimental design was used, first a full factorial followed by a central composite design (CCD). The CCD involved sulfuric acid (1.5% to 5%, v/v), a treatment at 121 ºC (15 min to 40 min), and varying CP content (10% to 20%, w/v). The response variables were the reducing sugars, glucose, and solubilized solids. Maximal responses were achieved at 3.4% (v/v) sulfuric acid, 20% (w/v) CP, and 22.3 min. A significant (R2 = 0.99) second-order model predicted maximal operational conditions that were experimentally validated: 80.1 g/L reducing sugars, 12.8 g/L glucose, and 69.2% solubilization of CP solids. The dilute sulfuric acid pretreatment solubilized all hemicellulose in CP.