Alumina supported NiMo nanocatalysts were synthesized through ultrasonic-assisted combustion method with various organic additives, including citric acid, ethylene glycol, glycine and urea using in hydrodesulfurization of thiophene at atmospheric pressure. The samples were characterized by XRD, TGA, FESEM, EDX, BET-BJH and TPR analyses. The results indicated that the type of organic compound has a noticeable effect on phase structure, surface morphology and reducibility potential as a consequence of different amount of heat and gaseous products released during combustion reaction. Our method showed that a relatively homogeneous distribution of the active material over the support can be achieved. Using citric acid as an organic additive, led to synthesis of nanocatalyst in which more than 90% of particles are less than 70 nm. The sample synthesized by citric acid exhibited the highest activity in hydrodesulfurization reaction due to its significant properties such as high surface area, considerable surface hole and weakened metal-support interaction compared with other organic additives. In addition, activity assessment of the prepared catalyst by ethylene glycol and glycine demonstrated that 100% abatement of thiophene can be achieved at 105 °C and 30 min.