The objective of this study was to evaluate the combination of physical and chemical pretreatments of wheat bran (WB) and oat hulls (OH) to obtain fermentable sugars and a residual solid fraction with increased susceptibility to enzymatic hydrolysis. High-pressure steam in an autoclave and ultrasonication were employed as pretreatments, and for both processes, WB and OH were treated with sulfuric acid (HSO), neutral medium (HO) and sodium hydroxide (NaOH). Autoclave high-pressure steam in an acid medium was the most effective for the release of sugars (total sugars, xylose and glucose) from liquid hydrolysates and for the modification of the residual solid fraction. The cellulose content of the WB residual solid fraction increased from 7.19 to 39.17%, the lignin fraction of WB decreased from 6.40 to 3.21%, the cellulose content of OH increased from 31.16 to 61.53%, and lignin fraction of OH decreased from 18.12 to 7.24%, resulting in materials more susceptible to enzymatic hydrolysis.