Yule Xie, Hongli Xia, Yi Ding, Yanchuang Zhao, Jiajian Peng, Xinxin Shao, Ying Bai
We report a Zn-enabled radical strategy for constructing aryl-alkyl diazo compounds from aryl diazonium salts and alkyl iodides. Zn serves as a simple single-electron transfer initiator to generate aryl radicals, which undergo rapid XAT to form alkyl radicals, followed by azo coupling. The method features a broad substrate scope, good functional group tolerance, and scalability. Notably, substrates capable of 1,5-HAT deliver C-H-functionalized products, highlighting the synthetic versatility of this protocol.