With the aim of exploring an alternative way to prepare Mo/Al2O3 catalysts, we concentrate our attention on Mo/boehmite systems with particular reference to the molybdenum localization at the boehmite interface and its influence on the boehmite to gamma-Al2O3 transformation. Several samples of boehmite at increasing Mo loading (0.02, 0.123 and 0.514 equivalent Mo/Al) have been synthesized and studied by means of diffuse reflectance infrared spectroscopy (DRIFTS), XRD and DTA-TGA. (C) 2003 Elsevier B.V. All rights reserved.