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A metal-free, visible-light driven C–H ketoalkylation of glycine derivatives and peptides with cycloalkyl hydroperoxides is presented. This protocol provides a straightforward route to unnatural amino acids bearing a distal carbonyl group with moderate to good yields. Preliminary mechanistic studies revealed that both a SET event and radical chain propagation were involved in this transformation.

Graphical abstract: Metal-free, visible-light driven C–H ketoalkylation of glycine derivatives and peptides

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