Sequential One‐Pot Rh(III)‐Catalyzed Direct C2 and C7 Alkylation of (Hetero)aromatic C—H Bonds of Indoles.

Abstract A simple and versatile method for highly efficient synthesis of various polysubstituted indoles via a sequential one-pot Rh(III)-catalyzed direct C2–H and C7–H alkylation with diazo compounds has been developed. This process features with mild reaction conditions, wide substrate scope, and good functional group tolerance (24 examples, up to 96% yield).