Photoelectrochemical Iron–Nickel Synergistic Catalysis for C(sp³)-H and Dehydroxymethylative Acylation

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We developed an iron–nickel dual-catalytic system for efficient C(sp 3 )-H activation acylation of hydrocarbons and carboxylic acids under photoelectrochemical conditions. This system is based on ligand-to-metal charge transfer-mediated direct hydrogen atom transfer and is applicable to inert C(sp 3 )-H-containing compounds. It also enables dehydroxymethylative acylation of alcohols, both these two reactions demonstrating broad substrate scope and unconventional chemoselectivity. Gram-scale synthesis, flow chemistry, and mechanistic studies highlight its potential in sustainable C(acyl)-C bond formation.