Alkaline oxidative fractionation of wood materials and sugarcane bagasse was performed either with or without of Cu-catalyst at 100 - 140 ºC for 5 or 24 h.  A fibre fraction with high enzymatic hydrolysability and a solubilised fraction containing recoverable lignin, hemicellulose, organic acids and some minor components were produced. Pretreatment was also efficient even without catalyst although the presence of the catalyst enhanced its performance. The enzyme dosage required for hydrolysis of the fibre was radically decreased as compared to materials obtained by steam explosion from the same raw materials. The demand of enzymes was decreased most significantly with long hydrolysis time, probably due to diminished inactivation and unproductive binding to the substrate. The binding of individual enzymes in total hydrolysis by cellulase mixture was studied by quantifying the purified major components of T. reesei cellulase system and A. niger β-glucosidase during hydrolysis of e.g. alkali oxidized and steam exploded spruce. These results clearly show the promise of the new method and motivate further development and scale up work.