The acid-catalyzed dehydration of D-xylose to furfural has been investigated in a biphasic water toluene system, using a mesoporous Nb2O5 catalyst prepared by a neutral templating route. The catalytic behavior was compared with a commercial Nb2O5. Materials were characterized by XRD, XPS, TEM, NH3-TPD, Raman spectroscopy and N-2 sorption. The D-xylose conversion and furfural yield over the mesoporous niobia were found to increase with reaction temperature and time, in such a way that at 170 degrees C and 90 min, a D-xylose conversion and a furfural yield were higher than 90% and 50%, respectively. However, the commercial crystalline niobia displayed a low activity. The stability of the mesoporous catalyst has been demonstrated by XRD and N-2 sorption, and corroborated by the absence of significant niobium leaching in solution. (C) 2014 Elsevier B.V. All rights reserved.