Pyridyl-Directed Cp*Rh(III)-Catalyzed B(3)–H Acyloxylation of o‑Carborane

An efficient pyridyl-directed Rh­(III)-catalyzed o-carborane B­(3)–H acyloxylation is reported. The B(3)–H bond is the most electron-deficient vertex on o-carborane whose functionalization is challenging. The combination of Cu­(OH)₂ and diverse carboxylic acids provides low cost and abundant acyloxyl sources which could lead to moderate to excellent yields.