The synthesis of 2, 5-diamino-1, 3, 4-thiadiazole derivatives was performed via the reaction of dithiocarbamate derivatives and hydrazine sulfate in presence of MgO nanoparticles as heterogeneous catalysts which were prepared by the sol-gel method. The pure products were produced in a simple and clean method in presence of MgO nanoparticles (5 mg) in the refluxing water (0.5 mL) around 10 hours with good to excellent yields (up to 95%). The prepared metal oxide nanoparticles were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and Fourier transform infrared (FT-IR) spectroscopy.