Dual C–H Functionalization of Tetrahydroisoquinolines and Tertiary Amines: A Unified Strategy for Direct α‐(2‐Oxoethylation) and Synthesis of Fused Aza‐Aromatic Architectures

A CBr₄‐mediated dual C–H functionalization strategy for the direct α‐(2‐oxoethylation) of N‐aryl tetrahydroisoquinolines (THIQs) with tertiary amines is disclosed. This atom‐economical process provides diverse aldehyde‐functionalized THIQs or, alternatively, ring‐opened α,β‐unsaturated aldehydes. Its utility is demonstrated by the concise construction of dihydroisoquinoline‐fused quinoline scaffolds, and preliminary studies indicate that these compounds exhibit good AIE activity, showing potential for further application in fluorescent materials.