A series of vanadium- and/or molybdenum-incorporated MCM-41 mesoporous materials was synthesized by rapid hydrothermal method. The synthesized mesoporous materials were characterized by XRD, N2 physisorption, TPR and EPR techniques. It is deduced from these characterization techniques that vanadium and/or molybdenum were incorporated into the framework of the MCM-41 structure. The extent of mesoporous structural ordering was evident from the XRD pattern of molybdenum and mixed MoV-MCM41. However, V-MCM-41 showed relatively less pronounced reflections for higher order peaks in XRD pattern. Catalytic results showed higher activity in case of mixed and V-MCM-41 catalyst as compared with Mo-MMAC-41 toward the oxidative dehydrogenation of n-butane in a fixed bed micro-reactor in the range of 500 to 600 °C at atmospheric pressure. Major products include ethylene, propylene and butenes along with substantial amount of pentene. A small amount of H2 was also produced during catalytic run under the conditions of catalyst performance evaluation.