This paper describes an organosolv pretreatment of corncob waste to improve its anaerobic digestion for biogas production. Through a thermochemical process based on the use of ethanol and acetic acid, it was possible to separate the fractions of lignin, considered to be a natural inhibitor of anaerobic digestion processes. In addition, with this organosolv pretreatment, the available sugars in the carbohydrates present as monosaccharides, or simple sugars, were depolymerised, facilitating the digestion process. The obtained results include the chemical characterisation of the corncob, the hydrolysate, and the mixture with cow manure, finding that these substrates have potential to be used in anaerobic digestion. The total reducing sugars consumed were 96.8%, and total sugars were 85.75%. It was clearly observed that with the use of pretreatment with organosolv, the production of biogas was superior, because 484 NmL/gVS was obtained compared to the other reported treatments. It was also observed that adding the hydrolysate organosolv increased the production because the values of the control without hydrolysate were 120 NmL/gVS in the bottle experiment. When the experiment was scaled to the 5L reactor, the total volumes of biogas that were accumulated in 15 days of production were 5050 NmL/gVS and 1212 NmL/gVS with and without hydrolysate, respectively. This indicates that the organosolv pretreatment of corncob waste is effective in improving biogas production.