The effect of a bis(proazaphosphatrane) ligand on the palladium‐catalyzed direct α‐arylation of nitriles with various aryl chlorides under mild conditions is reported. Comparisons of the catalytic properties of this ligand with those of three related mono(proazaphosphatrane)s under the same reaction conditions revealed that bis(proazaphosphatrane) displayed a synergistically enhanced activity. In the presence of the bis(proazaphosphatrane) ligand, ethyl cyanoacetate and primary as well as secondary nitriles were efficiently coupled with a wide variety of aryl chlorides that contained electron‐rich, electron‐poor, and electron‐neutral groups.

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Aw ide range of carboxylic acid derivatives including aldoximes, aldehydes, nitriles, primary amides, and carboxylic acid esters were reacted with various amines to form secondary and tertiarya mides from as ingle cobalt catalyst. CoCl 2 /PPh 3 wasr evealed as au niversal,e fficient catalystf or secondary or tertiary amide synthesis from av ariety of start-ing materials. At wo-step mechanism for the secondary amide synthesis from aldoximes was proposed and the substrate scope was intensively investigated. This study informs us about the reactivityo ft he cobalt catalystw ith regardst o carboxylic acid derivatives, along with the functional group tolerance of the substrates.[a] S.

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