The highly active Ni/Cu bimetallic nanoparticles (NPs) of the different molar ratios of Ni and Cu (1:1, 1:3, 3:1) assisted by dendritic ligand 2,4,6-Tris (di-4-chlorobenzamido)-1,3-diazine were synthesized successfully confirmed by Scanning Electron Microscopy (SEM), Electron Diffraction X-ray (EDX), X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), and Transmission Electron Microscopy (TEM) analysis. These NPs were studied as a heterogeneous catalyst for the chemoselective oxidation of alcohol to the corresponding aldehyde at 30 min and chemoselective reduction of aromatic nitro substituents to the corresponding amino substituents at 20 min, while the Ni/Cu (3:1) NPs were found to be the most effective among other Ni/Cu (1:1) and Ni/Cu (1:3) NPs at room temperature under mild conditions. The Ni/Cu (3:1) NPs can be recycled for at least five successive runs with no perceptible decrease in catalytic activity.