Nowadays, with increasing environmental concerns, the development of sustainable and friendly heterogeneous catalysts has attracted more and more attention in both the scientific and industrial communities. Hence, the use of nanocatalysts with well-defined structures, environmentally benign, high catalytic activity, and high chemical stability are desirable instead of corrosive and hazardous chemicals. In recent years, polymeric mesoporous graphitic carbon nitride (g-C₃N₄) has turned out to be a fascinating choice for catalyst or catalyst support due to the special physical and chemical properties, thermal stability, non-toxicity, unique electronic properties, and large surface area. The incorporation of nitrogen atoms in the carbon architecture of the g-C₃N₄ gives rise to the active chemical sites exposed on the surface. On the other hand, depositing metal nanoparticles onto g-C₃N₄ is an effective strategy to enhance the catalytic activity of g-C₃N₄. In the present study, g-C₃N­/Ni as a recyclable, highly efficient heterogeneous catalyst with a good porous structure have been prepared and its catalytic activity was investigated for the synthesis of quinoxaline derivatives.