Glycinamide‐Driven Coumarin Construction (GDCC): A Mild Strategy for Fluorescent Labeling and Macrocyclization of Peptides

X Xiao‐Fei Gao (jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China) W Wei Xiao (Center for Plant Molecular Biology, University of Tübingen) T Tian‐Ming Tao (National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China) F Feng‐Cai Ma (National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China) X Xiao‐Yan Liu (jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China) X Xue Jiang Z Zhong‐Hong Liu (jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China) X Xing‐Lei Zhang (Key Laboratory for Mass Spectrometry and Instrumentation East China University of Technology Nanchang China) Y Yu Chai (National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine) E Emeric Miclet (Sorbonne Université, Ecole Normale Supérieure, PSL University, CNRS, Laboratoire des Biomolécules, 4 place Jussieu, Paris Cedex 05, 75252, France) V Valérie Alezra (Laboratoire de Méthodologie, Synthèse et Molécules Thérapeutiques, ICMMO, Université Paris-Saclay) Y Yuan‐Biao Tu (National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China) Q Qi‐Dong Tu (jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China) Y Yang Wan (National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine) H Hai‐Sheng Wang (jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China) Q Qiang Xiao

Abstract

ABSTRACT Peptidic macrocycles have attracted increasing attention due to their well‐defined structures and enhanced biological activities. However, efficient cyclization of residues lacking reactive side chains remains a significant challenge. Herein, we report a glycinamide‐driven coumarin construction (GDCC) reaction that enables the in situ formation of coumarin scaffolds via condensation between C ‐terminal glycine residues and salicylaldehyde analogs under mild, metal‐ and catalyst‐free conditions. While various salicylaldehyde derivatives afford efficient fluorescent labeling, symmetrical salicylaldehyde‐based linkers uniquely promote intramolecular bis ‐glycine cyclization, generating intrinsically fluorescent peptide macrocycles with tunable topology and hydrophobicity. Notably, the optimal peptide 64 exhibits photophysical properties comparable or even superior to those of the coumarin gold standard, 7‐(diethylamino)‐4‐methylcoumarin. The GDCC reaction displays broad substrate scope and excellent compatibility with both solid‐phase and solution‐phase peptide synthesis. Its potential in chemical biology is demonstrated by the streamlined construction of diverse fluorescent cyclic peptides, including RGD‐based probes for live‐cell imaging, peptide–drug conjugates for targeted doxorubicin delivery, and a panel of PD‐1/PD‐L1 interaction inhibitors with tunable activity.

Article Details

Volume / Issue Vol. 65, Issue 17
Published April 20, 2026
ISSN 1433-7851
Publisher Wiley

Journal Info

Angewandte Chemie International Edition

Wiley

ISSN: 1433-7851 Physical Sciences

Authors (16)

X

Xiao‐Fei Gao

jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China

W

Wei Xiao

Center for Plant Molecular Biology, University of Tübingen

T

Tian‐Ming Tao

National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China

F

Feng‐Cai Ma

National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China

X

Xiao‐Yan Liu

jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China

X

Xue Jiang

Z

Zhong‐Hong Liu

jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China

X

Xing‐Lei Zhang

Key Laboratory for Mass Spectrometry and Instrumentation East China University of Technology Nanchang China

Y

Yu Chai

National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine

E

Emeric Miclet

Sorbonne Université, Ecole Normale Supérieure, PSL University, CNRS, Laboratoire des Biomolécules, 4 place Jussieu, Paris Cedex 05, 75252, France

V

Valérie Alezra

Laboratoire de Méthodologie, Synthèse et Molécules Thérapeutiques, ICMMO, Université Paris-Saclay

Y

Yuan‐Biao Tu

National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine Jiangxi University of Chinese Medicine Nanchang China

Q

Qi‐Dong Tu

jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China

Y

Yang Wan

National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine

H

Hai‐Sheng Wang

jiangxi Provincial Key Laboratory of Organic Functional Molecules, Institute of Organic Chemistry, College of Chemistry and Chemical Engineering Jiangxi Science and Technology Normal University Nanchang China

Q

Qiang Xiao