Anodic C(sp 3 )-H Acyloxylation of Indolin-3-ones Enabled by Oxidant-Free Cross-Dehydrogenative C(sp 3 )-O Coupling.

An efficient anodic C(sp 3 )-H acyloxylation protocol has been established via intermolecular cross-dehydrogenative C(sp 3 )-O coupling. The protocol provides various C2-acyloxy indolin-3-ones without the addition of metal catalysts and external oxidants because indolin-3-ones can be directly oxidized at the anode. The effective application of several medical drugs and the realization of the gram-scale experiment have proven the practicality of this protocol.