Formal Allylic C(sp <sup>3</sup> )−H Carboxylation With CO <sub>2</sub> via Copper Metallaphotoredox Catalysis

J Jun‐Ping Yue (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) H Huan‐Zhen Li (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) L Li‐Cai Liu (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) G Guang‐Rui Liu (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) Z Zu‐Tong Li (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) X Xin‐Yi Zhang (Faculty of Chemistry Northeast Normal University Changchun China) W Wen Wang J Jin‐Cheng Xu (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) L Lei Song H Hanjiao Chen (Analytical & Testing Center) X Xia Jiang (Department of Clinical Neuroscience, The Karolinska Neuroimmunology & Multiple Sclerosis Centre, Centre for Molecular Medicine, Karolinska Institutet) J Jian‐Bo Zhu (National Engineering Laboratory of Eco‐Friendly Polymeric Materials (Sichuan) State Key Laboratory of Advanced Polymer Materials College of Chemistry Sichuan University Chengdu P. R. China) S Si‐Shun Yan (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) J Jian‐Heng Ye (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China) D Da‐Gang Yu (Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China)

Abstract

ABSTRACT Catalytic carboxylation of ubiquitous C─H bonds with CO 2 has been demonstrated as a sustainable and streamlined pathway to valuable carboxylic acids. However, the catalytic carboxylation of abundant allylic C(sp 3 )─H bonds with CO 2 , which presents a unique opportunity to synthesize structurally diverse 3‐butenoic acids, still remains challenging. Herein, we report the first copper metallaphotoredox‐catalyzed formal allylic C(sp 3 )─H carboxylation with CO 2 , enabling efficient and selective synthesis of 3‐butenoic acids under mild and redox‐neutral conditions. This strategy lies in combining highly reducing photocatalysts to generate alkene radical anion intermediates with copper catalysis to orchestrate regioselective elimination, providing a distinct pathway from traditional allylic C(sp 3 )─H functionalization via forming allyl‐metal intermediates. This method features high atom and step economy, broad substrate scope, good functional group tolerance, facile scalability, and easy access to valuable compounds, including diverse bioactive molecules, natural products, and 13 C‐labeled anti‐inflammatory drug sulindac.

Article Details

Volume / Issue Vol. 65, Issue 22
Published May 25, 2026
ISSN 1433-7851
Publisher Wiley

Journal Info

Angewandte Chemie International Edition

Wiley

ISSN: 1433-7851 Physical Sciences

Authors (15)

J

Jun‐Ping Yue

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

H

Huan‐Zhen Li

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

L

Li‐Cai Liu

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

G

Guang‐Rui Liu

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

Z

Zu‐Tong Li

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

X

Xin‐Yi Zhang

Faculty of Chemistry Northeast Normal University Changchun China

W

Wen Wang

J

Jin‐Cheng Xu

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

L

Lei Song

H

Hanjiao Chen

Analytical & Testing Center

X

Xia Jiang

Department of Clinical Neuroscience, The Karolinska Neuroimmunology & Multiple Sclerosis Centre, Centre for Molecular Medicine, Karolinska Institutet

J

Jian‐Bo Zhu

National Engineering Laboratory of Eco‐Friendly Polymeric Materials (Sichuan) State Key Laboratory of Advanced Polymer Materials College of Chemistry Sichuan University Chengdu P. R. China

S

Si‐Shun Yan

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

J

Jian‐Heng Ye

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China

D

Da‐Gang Yu

Key Laboratory of Green Chemistry &amp; Technology of Ministry of Education College of Chemistry Sichuan University Chengdu P. R. China