The autohydrolysis process as a method for selective extraction of hemicelluloses and conversion to furfural was proposed for lignocellulosic raw materials. Samples of wheat straw (WS) and Eucalyptus globulus (EG) were subjected to nonisothermal autohydrolysis, defined by temperature 180–240°C. Within a biorefinery scheme for the selected materials, the aim of this study is both (a) to optimize furfural processing technology to enable higher yields and improved productivity from EG and WS by autohydrolysis and (b) to not excessively degrade the remaining polymeric constituents (glucan) in solid to facilitate a potential later use. Differences in the rate of the dehydration reaction of xylose to furfural have been observed, and it is faster in the case of WS with respect to that observed for eucalyptus. In that form, 4.25 g/100 g raw material (26% of the initial xylan in WS) could be found at 220°C, and an increase in the temperature (240°C) yielded 4.54 g/100 g raw material, 28% of the initial xylan. In EG, the increase in the hydrolysis temperature (240°C) yielded liquor with higher contents of furfural (4.45 g/100 g raw material, 25% of the initial xylan) and acetic acid (4.49 g/100 g raw material) and smaller contents of arabinose and xylan. In WS, a faster dehydration is found. © 2015 American Institute of Chemical Engineers Environ Prog, 34: 1236–1242, 2015