The widespread use of diesel in transportation, industry, and power generation leads to many environmental problems caused by high sulfur compound emissions. Diesel fuel must be free of sulfur-containing compounds due to their potential to cause severe environmental pollution. Oxidative desulfurization of diesel fuel using microwave irradiation technology is considered one of the most efficient methods to achieve this goal. This simple, economical, and effective approach for treating sulfur-containing diesel fuel employs peroxide oxidation facilitated by pimelic acid and heating through microwave radiation. The research sought to examine the effectiveness of the acid as a catalyst and hydrogen peroxide as an oxidizing agent. The technology relies on microwave electromagnetic radiation. A Central Composite Design (CCD) was used to plan experiments with three variables and five levels, and to analyze the effect of these variables on the desulfurization efficiency of diesel fuel. The results indicated that the highest efficiency for sulfur extraction from diesel fuel occurred at 400 W, with an optimal processing time of 150 seconds and a peroxide-to-diesel volume ratio of 0.5, achieving approximately 75% sulfur removal under these optimal conditions. Microwave technology thus represents an effective and cost-friendly environmental approach for sulfur removal from diesel fuel.