In this study, a nanostructured NdFeO₃ material was synthesized via a simple process of the hydrolysis of Nd (III) and Fe (III) cations in hot water with 5% NaOH as a precipitating agent. According to the results of the thermal behaviors of each hydroxide, either containing Fe (III) or Nd (III), the perovskite type of neodymium orthoferrite NdFeO₃ was simply synthesized by annealing a mixture of Fe (III) and Nd (III) hydroxides at 750 °C. The nanostructured NdFeO₃ was obtained in spherical granules with diameters of around 30 nm. The magnetic properties of the material were a coercive force (H_c) of 136.76 Oe, a remanent magnetization (M_r) of 0.68 emu·g^–1, and a saturation magnetization (M_s) of 0.79 emu·g^–1.