Regioselective Formal β-C(sp³)–H Amidation of Ketones by Merging Photocatalysis and Ni-Nitrenoid Transfer

β-Amino carbonyls are synthetically valuable scaffolds that are prevalent in bioactive molecules and pharmaceuticals, yet efficient and selective methods for their synthesis remain underdeveloped. Disclosed herein is a dual photoredox/nickel-catalyzed platform for the formal β-C(sp³)-H amidation of ketones to access β-amido ketones. The method enables the regioselective β-amidation of both cyclic and linear ketones under mild conditions, employing silyl enol ethers and dioxazolones as readily available coupling partners. Mechanistic studies support the involvement of a photogenerated allylic carbon radical, which engages with Ni-nitrenoid species to facilitate C(sp³)-N bond formation.