Sonochemical preparation of Co and Ni promoted MoS2 Supported on alumina was achieved by high-intensity ultrasonic irradiation of isodurene solutions containing molybdenum carbonyl, dicobalt octacarbonyl, elemental sulfur, and Al2O3 or Ni-Al2O3 under Ar flow. The sonochemically prepared catalysts were characterized by elemental analysis, XPS, SEM, TEM, and XEDS, and hydrodesulfurization (HDS) activity evaluated for thiophene and dibenzothiophene substrates. The TEM studies on the sonochemically prepared catalysts indicate the formation of layered hexagonal MoS2 (lattice fringes similar to6.2 Angstrom) on the alumina support. The sonochemically prepared Co-Mo-S/Al2O3, Ni-Mo-S/Al2O3, and Co-Ni-Mo-S/Al2O3 are extremely active catalysts for the HDS of thiophene and dibenzothiophene, with activities severalfold those of comparable commercial catalysts under identical conditions. The layered structure Of MoS2 remained intact after 120 h of HDS, and the catalyst is reusable.