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A single-atom iron catalyst was found to exhibit exceptional reactivity in acceptorless dehydrogenative coupling for quinoline synthesis, outperforming known homogeneous and nanocatalyst systems. Detailed characterizations, including aberration-corrected HAADF-STEM, XANES, and EXAFS, jointly confirmed the presence of atomically dispersed iron centers. Various functionalized quinolines were efficiently synthesized from different amino alcohols and a range of ketones or alcohols. The iron single-atom catalyst achieved a turnover number (TON) of up to 10
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