The catalytic performance of unsupported Me/MoS2 catalysts (where Me = Co, Ni, Fe) in the hydrotreating reactions of furfurylamine (FA) and dibenzothiophene (DBT) in a dynamic micro-reactor was reported. The Me/MoS2 samples were synthesized by the impregnated thiosalt decomposition (ITD) method and sulfided under a mixture H2S/H2 (20% v/v), at 400 °C for 4 h. In all samples the Me/(Me + Mo) atomic ratio was of 0.85. The samples were characterized by Chemical analysis by EDS, N2 adsorption–desorption, X-ray diffraction, X-ray photoelectron spectroscopy, and high-resolution transmission electron microscopy. The Ni/MoS2 sample showed higher catalytic activity in the hydrotreating reactions of FA and DBT in comparison with the Co/MoS2 and Fe/MoS2 samples. The selectivity in both FA and DBT reactions depends strongly on the presence of Me (Ni, Co or Fe). We found two interesting correlations between the catalytic activity of both FA and DBT reactions with the fraction sulfided of Me and Mo species and with the total sulfidation degree of the samples.