Remote Selective Cross‐Dehydrogenative Coupling Reactions of Aryl C–H Bonds with Carboxylic Acids at Room Temperature

An efficient Pd(II)‐catalyzed remote selective cross‐dehydrogenative coupling of broadly useful synthetic building blocks biphenyl Weinreb amides with carboxylic acids is developed. This acetoxylation protocol is performed under room temperature using N‐fluorobenzene‐sulfonimide (NFSI) as the oxidant, exhibiting a wide range of functional group tolerance and affording δ‐position‐ selective products up to 85% yield. Notably, a diverse set of carboxylic acid‐containing drugs is also found to be compatible under the current reaction conditions. Preliminary mechanistic studies indicate that this reaction presumably proceeds through a seven‐membered palladacycle intermediate.