The design and synthesis of a new nanostructured material that can efficiently catalyze selective reduction reactions in an eco‐friendly way is an active area of research today. Here a mesoporous Ni–Al mixed oxide material has been synthesized hydrothermally by using lauric acid as capping agent. The mesoporosity observed in the material is mainly originated from the interparticle voids created due to the self‐assembly of the nanoparticles (NPs) in the presence of capping agent used during the synthesis. The material has been characterized by powder XRD, N2 sorption, high‐resolution transmission electron microscopy (HRTEM), scanning electron microscopy/energy‐dispersive spectroscopy (SEM‐EDS), FTIR, and thermogravimetric/differential thermal analysis (TG‐DTA) tools. The mesoporous Ni–Al mixed‐oxide material showed a very high Brunauer–Emmett–Teller (BET) surface area (337 m2 g–1) and excellent catalytic activity in a selective liquid‐phase hydride‐transfer reduction reaction of nitroarenes to their corresponding anilines in the presence of 2‐propanol as hydride source.