Fe^III/TBHP‐Driven Radical Activation of Methanol: A Green and Renewable C1‐Feedstock for Sustainable Synthesis of <i>N</i>‐Heterocycles at Room Temperature

Abstract To address the issues of climate change and energy crises, it is vital to overhaul energy and chemical manufacturing processes, focusing on environmentally sustainable practices that are practical and widely adoptable. As a contribution to this goal, we herein present an earth‐abundant Fe‐catalyzed, radical‐driven strategy for the challenging activation of methanol, a green and renewable C1 feedstock, for the efficient synthesis of quinoline scaffolds under room temperature conditions. The developed transformation involves Fe III /TBHP‐mediated radical activation of methanol to generate a C1 synthon, which subsequently couples with arylamines, followed by C─H annulation with alkynes to yield the corresponding quinolines. By employing this efficient domino process, a diverse range of substituted quinolines were synthesized with excellent yields. The value of this multitasking protocol has been demonstrated through its broad substrate scope, excellent scalability and synthetic applications.