A General Electrochemical Platform for Dehydrazinative Oxygenation of Hydrazines

Herein, we disclose an electrochemical protocol that operates under catalyst‐free conditions at room temperature, enabling the dehydrazinative oxygenation of hydrazines with TEMPO. This straightforward approach relies on anodic oxidation to initiate a radical pathway, furnishing a diverse array of C─O coupling products in satisfactory yields. The transformation accommodates a wide range of hydrazine derivatives, showcasing outstanding tolerance toward various functional groups. The preparative utility of this method is further demonstrated by late‐stage functionalization of bioactive compounds, gram‐scale reactions, and subsequent product modifications. Mechanistic studies indicate that the process proceeds through an electrochemically driven radical coupling pathway.