The main goal of this research is to evaluate the effects of various parameters on the synthesis of a Fe−Mo catalyst supported on an in-house developed mesoporous activated carbon. For this purpose, mesoporous carbon has been prepared from grape branches and oil palm trunks under various activation times and drying periods. Consequently, optimum values of the aforementioned parameters have been obtained in order to synthesize an efficient support for developing a heavy naphtha hydrodesulfurization (HDS) catalyst. Subsequently, a mixture of Fe−Mo with a weight ratio of 1:3 has been loaded on the developed supports through a wet impregnation method. Various experimental analyses including X-ray diffraction (XRD), Fourier transform infrared (FTIR), Brunauer−Emmett−Teller (BET), temperature programmed desorption (TPD), temperature programmed reduction (TPR), field-emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), X-ray fluorescence (XRF), thermogravimetric analysis (TGA), and energy dispersive X-ray (EDX) have been undertaken to determine the characteristics of synthetic catalysts and activated carbons. Once an appropriate catalyst has been synthesized on the basis of the experimental analyses, its performance for hydrodesulfurization of heavy naphtha has been investigated and has been compared to the efficiency of a catalyst with a commercial activated carbon support. The obtained results reveal that the sulfur conversions of heavy naphtha containing 900 ppm sulfur compounds at atmospheric pressure and at 340 °C are around 78 and 55% for the desulfurization process using the synthesized catalyst in the present work and the used commercial catalyst, respectively. It has also been found that a combination of grape branches and oil palm trunks contributes to an efficient mesoporous carbon structure, an acceptable thermal stability, and the development of a cost-effective support for the synthesis of an industrially viable HDS catalyst.