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Organophosphonium salts containing C(sp3)−+P bonds are among the most utilized reagents in organic synthesis for constructing C−C double bonds. However, their use as C‐selective electrophilic groups is rare. Here, we explore an efficient and general transition‐metal‐free method for sequential chemo‐ and regioselective C−H and C(sp3)−+P bond functionalizations. In the present study, C−H alkylation...
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