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Mixed Ni-Al oxide catalytic precursors with different elemental ratios (20, 50, and 80 wt.% Ni⁰) were synthesized using green supercritical antisolvent co-precipitation (SAS). The obtained oxide precursors and metal catalysts were characterized in detail by X-ray diffraction (XRD) analysis, atomic pair distribution function (PDF) analysis, CO adsorption, and high-resolution transmission electron microscopy (HRTEM). It was found that the composition and structure of the Ni-Al precursors are related to the Ni content. The mixed Ni_1−xAl_xO oxide with NiO-based crystal structure was formed in the Ni-enriched sample, whereas the highly dispersed NiAl₂O₄ spinel was observed in the Al-enriched sample. The obtained metal catalysts were tested in the process of anisole H₂-free hydrogenation. 2-PrOH was used as a hydrogen donor. The catalyst with 50 wt.% Ni⁰ demonstrated the highest activity in the hydrogenation process.