Rhoda‐Electrocatalyzed Bimetallic C−H Oxygenation by Weak O ‐Coordination

Rhodium‐electrocatalyzed arene C−H oxygenation by weakly O ‐coordinating amides and ketones have been established by bimetallic electrocatalysis. Likewise, diverse dihydrooxazinones were selectively accessed by the judicious choice of current, enabling twofold C−H functionalization. Detailed mechanistic studies by experiment, mass spectroscopy and cyclovoltammetric analysis provided support for an unprecedented electrooxidation‐induced C−H activation by a bimetallic rhodium catalysis manifold.