Zeyu Hu, Jia‐Hong Wu, Liejin Zhou, T T Wang
Abstract By merging gold catalysis with tetrapeptide-based bis-quaternary phosphonium salts, we have developed a relay catalytic system for the enantioselective synthesis of chiral azepines via a cascade 1-aza-Cope rearrangement of dienyne amides and α-bromophosphonoacetates. This strategy uniquely integrates a ring-opening process during the rearrangement, enabling efficient stereochemical transfer and facilitating product formation. Using this approach, a diverse array of chiral azepines was synthesized in excellent yields (up to 96%) with outstanding stereoselectivities (up to 98% ee and >20:1 dr).