The processes of xylose dehydration and the consecutive furfural hydrogenation have been combined in a single biphasic reactor. The dehydration was studied over Amberlyst-15 and the hydrogenation over a hydrophobic Ru/C catalyst. 1-Butanol, 2-methyltetrahydrofuran and cyclohexane were used as solvents in the process. The hydrogenation catalyst in the reactor was present in the organic phase and the dehydration catalyst in the aqueous phase. An increase of the hydrophobicity of the solvent in the order 1-butanol <2-methyltetrahydrofuran <cyclohexane suppressed the hydrogenation of xylose to xylitol due to a decrease of the xylose solubility, while forming furfural hydrogenation products. The main product is tetrahydrofurfuryl alcohol.