Synthesis of α‐Nitroketones through Electrochemical Olefin Oxidation–Nitration

Comprehensive Summary Herein, we report an environmentally friendly electrochemical method for the synthesis of α‐nitroketones from olefins. In this approach, Fe(NO 3 ) 3 ·9H 2 O and trace amounts of H 2 O in the system serve as nitrogen and oxygen sources, respectively, enabling the formation of α‐nitroketones through an oxidation–nitration reaction with olefins. This method eliminates the requirement for condensation reagents and nitromethane, thus providing a green and sustainable alternative. The reaction proceeds under mild conditions, exhibits a broad substrate scope, and demonstrates excellent functional group tolerance. Moreover, the protocol is cost‐effective, highly compatible, and easily scalable for large‐scale synthesis.