In this study, electrochemical oxidation of methanol to formic acid using the economical and highly active catalytic Nickel Benzene tricarboxylic acid metal organic framework (Ni-BTC-MOF) and reduced graphene oxide (rGO) nanocomposites modified glassy carbon electrode GCE in alkaline media, which was examined via cyclic voltammetry technique. Nickel based MOF and rGO nanocomposites were prepared by solvothermal approach, followed by morphological and structural characterization of prepared samples through X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), and energy dispersive X-ray (EDX) analysis. The electrochemical testing of synthesized materials represents the effect of the sequential increase in rGO concentration on electrocatalytic activity. The Ni-BTC/4 wt % rGO composite with a pronounced current density of 200.22 mA/cm2 at 0.69 V versus Hg/HgO electrode at 50 mV/s was found to be a potential candidate for methanol oxidation in Direct Methanol Fuel Cell (DMFC) applications. Product analysis was carried out through Gas Chromatography (GC) and Nuclear Magnetic Resonance (NMR) spectroscopy, which confirmed the formation of formic acid during the oxidation process, with approximately 62% yield.