Acylation of Csp2-H bond with acyl sources derived from alkynes: Rh-Cu bimetallic catalyzed C[triple bond, length as m-dash]C bond cleavage.

A Rh-Cu bimetallic catalyzed o-acylation of acyloxacetamide with alkynes has been described. This transformation provides a novel, concise way to synthesize ortho-acylphenols using functionalized alkynes as acylating reagents. Mechanistic studies revealed a Rh-Cu relay process, in which O2 plays a critical role for the formation of carbonyl compounds.