Summary Graphitic carbon nitride is of interest for its intercalation, ion exchange, and redox properties as it exhibits high catalytic activity. Besides, its high nitrogen content and facile synthesis procedure may provide a good balance between activity and durability. We report novel g‐C3N4 based MOF as a novel electrocatalyst for methanol oxidation reaction (MOR). Two methods are involved in the catalytic synthesis, namely the hydrothermal method for the Cu/Ni MOF and its composites synthesis, and g‐C3N4 is obtained by pyrolysis of melamine. To explore the structural and morphological properties, all the catalysts were eventually characterized using XRD, FTIR, SEM, and EDX techniques, whereas cyclic voltammetry (CV) revealed the electrochemical response for the oxidation of methanol in 3 M methanol and 1 M NaOH on modified glassy carbon electrode (GCE). The electrochemical results illustrate that as the amount of g‐C3N4 increases current density for methanol oxidation reaction (MOR). The maximum current density is 103.42 mA/cm2 shown by Cu/Ni MOF@5 wt% g‐C3N4 at 0.9 V while the scan rate is 50 mV/s. Thus, graphitic carbon nitride addition in MOF composites enhanced its durability and high carbon monoxide (CO) tolerance makes active catalysts in alkaline electrolyte.