Yellow-Light-Mediated Synthesis of Amidoximes via Radical <i>gem</i> -Diamination of Diazo Compounds

<i>N</i>-Nitrosamines serve as bifunctional reagents to install both amino and nitroso groups across unsaturated bonds, yet their use as diamine reagents remains underdeveloped. Herein, we introduce a simple yellow-light-driven reaction that directly forms amidoximes from <i>N</i>-nitrososulfonamides and diazo compounds. The process works by selectively activating the N-NO bond with low-energy light (λ > 590 nm), thereby avoiding side reactions and ensuring high selectivity.