Nanoscale, high surface area bulk molybdenum nitrides have been synthesized using two methods : a laser pyrolysis technique (LPT) and a temperature-programmed reaction (TPR). The activities of these materials for the simultaneous hydrodenitrogenation (HDN) and hydrodesulfurization (HDS) of Illinois No. 6 naphtha were determined. Both catalysts were active for the HDN and HDS reactions and, on an unit mass basis, exhibited the same activity and selectivity.