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Diversity-Oriented Synthesis of Azepinoindoles through sp <sup>3</sup> C–H Functionalization and Skeletal Remodeling

Yao‐Bin Shen, Fen Ma, Hao-Qi Song, Bin Qiu, Xiao‐De An, Houchen Wang, Tiesheng Shi, Zhihui Hao, Jian Xiao

2025Organic Letters14 citationsDOI

Abstract

Molecular editing of N-heterocycles represents a powerful strategy for enhancing compound complexity and structural diversity at a late stage. However, combining both peripheral and skeletal editing of pyrrolidines for the diversity-oriented synthesis of azepinoindoles remains underexplored yet challenging. Herein, we report the ethanol-mediated redox sp 3 C–H functionalization of pyrrolidines via the tert -amino effect and trifluoroacetic acid-promoted skeletal remodeling involving pyrrolidine ring expansion, which enables the divergent synthesis of azepino[4,3,2- cd ]indoles and azepino[2,3- e ]indoles. This method expands the scope of molecular editing of pyrrolidines, featuring metal-free reaction conditions, excellent functional group compatibility, late-stage modification of drug molecules, scalability, operational simplicity, and product derivatization. The mechanistic studies corroborate the proposed reaction pathway.

Topics & Concepts

ChemistryPyrrolidineSurface modificationCombinatorial chemistryPosttranslational modificationFunctional diversityFunctional groupScope (computer science)Ring (chemistry)StereochemistrySmall moleculeRetrosynthetic analysisDrug discoveryReaction conditionsChemical biologyRedoxNatural productBioorthogonal chemistryMoleculeTrifluoroacetic acidBiochemistryTrifluoroacetic anhydrideChemical synthesisCatalytic C–H Functionalization MethodsRadical Photochemical ReactionsSynthesis and Catalytic Reactions
Diversity-Oriented Synthesis of Azepinoindoles through sp <sup>3</sup> C–H Functionalization and Skeletal Remodeling | Litcius