Mesoporous Nb-MCM-41 molecular sieves (Si/Nb = 50 and 75) were synthesized hydrothermally. As-synthesized and calcined catalysts were characterized by low angle X-ray powder diffraction (XRD), N2-adsorption isotherm, thermogravimetric and FT-IR techniques. The niobium impregnated MCM-41 catalysts were also prepared by wet method and their structure was elucidated XRD and FT-IR spectroscopy. Electron spinning resonance (ESR) studies conformed the co-ordination environment of niobium in both type of catalysts. The catalytic activity of the above catalysts was studied for the vapor phase oxidation ofm-toluidine with CO2-free air at 200, 250, 300, 350, 400 °C. The major products werem-aminobenzoic acid andm-aminobenzaldehyde. Them-toluidine conversion was found to be higher in niobium impregnated catalysts than incorporated catalysts. The selectivity tom-aminobenzoic acid, which was the principally aimed product in this study, was found to be higher than that of them-aminobenzaldehyde. The activities of catalysts follow the order Nb-MCM-41 (1%)>Nb-MCM-41 (2%)>Nb-MCM-41 (3%)>Nb-MCM-41 (50)>Nb-MCM-41 (75). The effect of weight hourly space velocity and time on stream was also studied on conversion and products selectivity and the results are discussed. Conditions were optimized for betterm-toluidine conversion and products selectivity. [ABSTRACT FROM AUTHOR]