Synthesis and Functionalization of π‐Extended [7]Carbohelicene

ABSTRACT Helicenes represent a unique class of chiral molecular scaffolds with significant potential in multifunctional materials. Herein, we report the efficient synthesis and characterization of a novel [7]helicene derivative, [7]‐OTf , bearing reactive triflate groups. X‐ray crystallography confirms the helical structure and enantiomer stacking of [7]‐OTf , while a high racemization barrier of 46.5 kcal·mol −1 enables the chiral separation by high‐performance liquid chromatography. [7]‐OTf exhibits green emission ( λ em = 487 nm) with a quantum yield of 20% and mirror‐image chiroptical responses. Importantly, post‐synthetic modification was successful via Sonogashira coupling. This work establishes [7]‐OTf as a versatile and modifiable platform for advanced chiral materials.