Olive tree leaves, an abundant agricultural by-product without enough industrial market outlets, are presented in this study as a relevant resource of available carbohydrates to be chemically treated for monomeric sugar production. Characterization of two main granulometric fractions is the starting point for testing the specific effect and the relevance of three main factors (time, temperature, and sulfuric acid concentration) on diluted acid hydrolysis with respect to oligosaccharides, simple sugars, and fermentation inhibitory compounds production. The selected conditions (100 ∘ C, 90 min, and 6% w/w H 2 SO 4 ) to perform the small scale hydrolytic process, considering response surface methodology (2 3 factorial design with center points), implied production of acetic acid and hydroxymethylfurfural in concentrations not exceeding 1.10 kg m − 3 and 0.25 kg m − 3 , respectively. Thus, these experimental conditions were the reference framework to evaluate the effect of a meaningful scaling stage in a hydrolysis reactor, considering kinetic parameters based on hydrolysis rates and d-glucose and d-xylose generation.