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Noble‐metal nanocatalysts are quite popular, but the use of magnetic catalysts composed of ferrite materials is rare. Here, we have synthesized transition‐metal‐based cube‐shaped nanoparticles of approximately 11 nm in size, the so‐called magnetic nickel ferrite nanocatalyst (NFNC), by a new method and shown its use in the reduction of nitroaromatic compounds. The NFNC was characterized by using XRD, energy‐dispersive X‐ray spectroscopy, TEM, and field‐emission SEM to confirm the structural features and morphology of the particles. The catalytic activity of NFNC was investigated in the reduction of 4‐nitrophenol to 4‐aminophenol by monitoring the reaction by using UV/Vis spectroscopy. The catalytic activity, recyclability and reusability, rate constant of the reaction, and surface area were investigated in detail to understand the catalytic phenomenon. We measured up to 30 cycles of the catalytic reaction using our NFNC, which shows the high stability of the catalyst. BET analysis of the NFNC shows a surface area of 54.60 m2 g−1. Our NFNC has many advantages because it is prepared easily, cost effective, highly stable, and environmentally compatible. The magnetic properties of the NFNC help us to separate the particles easily after its use in the reduction without disturbing the final product.

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