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Highly efficient, one‐step synthesis of sulfur‐containing heteroacenes was achieved through palladium‐catalyzed C−S cross‐coupling of bis‐alkynes with thioacetate as hydrogen sulfide surrogate. Heteroacenes consisting of three, five, and seven fused aromatic rings were obtained in a single catalytic step by four‐, six‐, and eightfold C−S bond formation.
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