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Herein is reported a Rh2(OAc)4/IMes ⋅ HCl system that promotes the chemoselective installation of aryl groups at the 2‐position of furo[2,3‐b]pyridine (53–94% yields). The method is applicable to the direct modification of the natural furoquinoline alkaloid dictamnine. The cardiac effects of the fluorinated analogues improved, compared to dictamnine at 160 μg/mL. Preliminary mechanism of action studies...