Dual HATs‐mediated Catalyst‐free sp3 C‐H Bond Functionalization for Regioselective Radical Hydroalkylation of Ynazoles

Direct hydroalkylation of ynazoles, facilitating the efficient synthesis of linear N‐β‐vinylazoles, is accomplished through the functionalization of sp3 C‐H bonds using trace amounts of dioxygen as an initiator. This reagent‐free method eliminates the need for exogenous reagents and proceeds through a radical chain mechanism involving dual hydrogen atom transfer (HAT) processes. Its application potential is exemplified through the implementation of scale‐up operations.