Carbon-containing MoS2 catalysts with specific surface areas of up to 32.4 m(2)/g are prepared in situ from ethylenediammonium thiomolybdate (EtDaT, n= 2), 1,4-butane-diammonium thiomolybdate (BuDaT, n=4), 1,6-hexanediammonium thiomolybdate (HeDa, n=6), and 1,8-octanediammonium thiomolybdate (OcDaT, n=8), where BuDaT and OcDaT are novel precursors. The n-methylenediammonium thiomolybdates are prepared by reacting ammonium thiomolybdate (ATM) with ethylenediamine, 1,4-butanediamine, 1,6-hexane-diamine and 1,8-octanediamine, respectively, in an aqueous medium containing NH4Cl. Catalysts, as characterized by XRD and TEM, present a well-dispersed 2H-MoS2 phase. For the hydrodesulfurization (HDS) of dibenzothiophene (DBT), their first order rate constants, k, are more than two times higher than that of the reference catalyst (32.0 x 10(-7) mol/g s) derived from carbon-free ATM, with the MS-HeD catalyst being the most active k=86.3 x 10(-7) mol/g s. (C) 2014 Elsevier B.V. All rights reserved.