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A regioselective C8−H alkylation strategy with inert alkyl chloride on polyaromatics has been reported. Inexpensive transition metals nickel and cobalt enable access to various C8‐substituted polyaromatic products with good yields, suggesting a potential late‐stage functionalization of naphthalene‐based natural products and bioactive molecules. In the two‐phase mechanism, cobalt is responsible for radical generation, and nickel undergoes the C8−H insertion. More details are discussed in the article by Zhang and Mao et al. on pages 1121—1128. image