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Nano-sized crystal materials of NiAl2O4 metallic doped catalyst has been productively created by sol-gel combustion manner with the proper proportions of glycine supported nickel nitrate, alumnium nitrate and heated under the highest temperature on 900ºC performed into the muffle furnace. The structural, morphological, and spectral properties have been examined by using FT-IR, EDS, and FESEM study exposed to the formation of crystalline NiAl2O4 Nano-particles. This afforded metals catalyst has been employed as a catalyst in the synthesis of different substituted amine derivatives by conventional methods. It was found that the highest yield acquired in the synthesis of the N-substituted formamide derivatives by the application of nickel aluminate nano-catalyst.