EDA Complex–Mediated C(sp ³ )–H Cross‐Dehydrogenative Coupling Enables Synthesis of Noncanonical <i>α</i> , <i>β</i> ‐Diamino Acids

Nonproteinogenic α , β ‐diamino acids are key motifs in bioactive compounds. We report a photoinduced cross‐dehydrogenative coupling (CDC) of N ‐arylglycine derivatives with amides. This reaction proceeds via an electron donor–acceptor (EDA) complex that enables regioselective C(sp 3 )–C(sp 3 ) cross‐coupling, providing access to non‐canonical α , β ‐diamino acids from simple precursors.