The importance of HMF oxidation lies in its pivotal role as an intermediate in the sustainable synthesis of FDCA, a high-value chemical with diverse applications. This work presents a facile hydrothermal synthesis method for the preparation of a NiFeMo-alloy on nickel foam, subsequently annealed in an Ar/H2 mixed flow gas. Comparative studies were conducted by preparing bimetallic alloys (NiFe, NiMo, FeMo) under the same conditions. The resulting electrodes were employed as electrocatalysts for the oxidation of 5-hydroxymethylfurfural (HMF) to 2,5-furandicarboxylic acid (FDCA). Among the bimetallic alloys, NiFeMo exhibited superior electrocatalytic activity, achieving an impressive HMF conversion rate of 96.5%. The synergistic effects of Ni, Fe, and Mo in the alloy contribute to enhanced catalytic activity, demonstrating the potential of NiFeMo as a catalyst for sustainable and economically viable chemical transformations.