Potassium‐Sodium Co‐ doped Carbon Nitride for Enhanced Visible‐Light‐Driven Heterogeneous Photocatalytic Hydroalkylation of Arylazo tert ‐Butyl Carboxylates

A visible‐light‐responsive potassium‐sodium co‐doped carbon nitride (KNa‐CN) is successfully synthesized through elemental doping. The material is thoroughly characterized, revealing that the incorporation of potassium and sodium effectively narrows the band gap and significantly improves the separation efficiency of photogenerated charge carriers. Under visible light irradiation, KNa‐CN exhibits excellent catalytic performance in radical addition reactions, enabling the construction of C–N bonds via the reaction of arylazocarboxylic tert ‐butyl esters with N , N ‐dimethylanilines to produce N ′‐Boc‐ N ′‐alkyl‐ N ‐aryl hydrazine derivatives, with high regioselectivity and broad functional group tolerance. Moreover, the catalyst demonstrates high efficiency at the gram scale and retains its activity over three consecutive cycles without significant degradation.