-Due to ever more severe environmental regulations regarding SOx, NOx and other pollutants' emissions, there has been an interest in developing new and improved catalysts for hydroprocessing reactions. Mo2C has been reported to display good selectivity and activity for those reactions, especially for HDS. Addition of another metal to the carbide structure may improve catalytic properties. Mo2C with low cobalt addition (2.5 and 5%) was obtained via gas-solid reaction in a fixed bed reactor with CH4 (5%)/H2 atmosphere. XRD and TG/DTA analysis of the precursors were carried out in order to understand its mass loss profile, doping metal presence and phase distributions. CoMoO4 as well as MoO3 were identified after calcining doped precursors at 600 °C/180min. SEM, XRD, XRF, TOC, BET and laser granulometric analysis of the reaction products were also performed. Compositions verified by XRF and theoretical values were compatible. At 700 °C both carbide (Mo2C) and oxide (MoO2) phases are present, as identified in XRD analysis and observed by SEM. At 750 °C only single phase Mo2C was verified by XRD, indicating Co dispersion on the carbide matrix. Morphology at this temperature is compatible with pure Mo2C, though XRF indicates Co presence on the material.