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Developing catalytic approaches to selective activation and functionalization of C–H bonds in hydrocarbons and complex organic molecules has been considered as a challenging goal. Recently, significant efforts have been aimed at the search for efficient nickel‐ and palladium‐based catalyst systems, capable of conducting direct aliphatic C–H oxygenation with high and predictable chemoselectivity and regioselectivity. The present review focuses on the advances in homogeneous oxidation of hydrocarbon C(sp3)–H groups, catalyzed by nickel and palladium complexes, and covers the publications of the past 15 years. Correlations between the structure of the metal‐based catalyst, steric and electronic properties of the ligands, catalytic conditions, and the catalytic reactivity (efficiency, chemoselectivity, and regioselectivity) are discussed.