Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization

Abstract Introducing distinctive functional groups to expand the structural diversity and improve the intrinsic properties of parent molecules has been an essential pursuit in organic chemistry. By using perfluoroalkyl halide (PFAH) as a nontraditional, readily available, ideal 1,2‐difluoroalkenyl c...

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Main Authors: Yu‐Lan Chen, Wei Han, Yuan‐Yuan Ren, Mengtao Ma, Danhua Ge, Zhi‐Liang Shen, Kai Guo, Xue‐Qiang Chu
Format: Article
Language:English
Published: Wiley 2025-02-01
Series:Advanced Science
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Online Access:https://doi.org/10.1002/advs.202404738
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author Yu‐Lan Chen
Wei Han
Yuan‐Yuan Ren
Mengtao Ma
Danhua Ge
Zhi‐Liang Shen
Kai Guo
Xue‐Qiang Chu
author_facet Yu‐Lan Chen
Wei Han
Yuan‐Yuan Ren
Mengtao Ma
Danhua Ge
Zhi‐Liang Shen
Kai Guo
Xue‐Qiang Chu
author_sort Yu‐Lan Chen
collection DOAJ
description Abstract Introducing distinctive functional groups to expand the structural diversity and improve the intrinsic properties of parent molecules has been an essential pursuit in organic chemistry. By using perfluoroalkyl halide (PFAH) as a nontraditional, readily available, ideal 1,2‐difluoroalkenyl coupling partner, a defluorinative cyclization reaction of enamides for the construction of fluoroalkenyl oxazoles is first developed. The selective and controllable two‐fold cleavage of vicinal C(sp3)─F bonds in PFAH not only enables the introduction of a specific 1,2‐difluoroalkenyl moiety with ease but also results in the functionalization of two C(sp2)─H bonds of enamides without the need for metal catalyst, photocatalyst, oxidant, or light. The method can be applied to the late‐stage modification of complex molecules, synthesis of biological‐relevant oxazole analoges, and scale‐up synthesis, which all further highlight the real‐world utility of this protocol. Mechanistic studies reveal that the reaction possibly proceeds through a radical perfluoroalkylation, consecutive C─F bond heterolytic cleavage, and cyclization process. In addition, the in situ formed perfluoroalkyl radical which may also serve as an essential hydrogen abstractor.
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spelling doaj-art-7aa3592db4e444b4bbe29686ddba7cb82025-08-20T02:30:35ZengWileyAdvanced Science2198-38442025-02-01128n/an/a10.1002/advs.202404738Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds FunctionalizationYu‐Lan Chen0Wei Han1Yuan‐Yuan Ren2Mengtao Ma3Danhua Ge4Zhi‐Liang Shen5Kai Guo6Xue‐Qiang Chu7Technical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaTechnical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaTechnical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaDepartment of Chemistry and Materials Science College of Science Nanjing Forestry University Nanjing 210037 ChinaTechnical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaTechnical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaCollege of Biotechnology and Pharmaceutical Engineering Nanjing Tech University Nanjing 211816 ChinaTechnical Institute of Fluorochemistry School of Chemistry and Molecular Engineering Nanjing Tech University Nanjing 211816 ChinaAbstract Introducing distinctive functional groups to expand the structural diversity and improve the intrinsic properties of parent molecules has been an essential pursuit in organic chemistry. By using perfluoroalkyl halide (PFAH) as a nontraditional, readily available, ideal 1,2‐difluoroalkenyl coupling partner, a defluorinative cyclization reaction of enamides for the construction of fluoroalkenyl oxazoles is first developed. The selective and controllable two‐fold cleavage of vicinal C(sp3)─F bonds in PFAH not only enables the introduction of a specific 1,2‐difluoroalkenyl moiety with ease but also results in the functionalization of two C(sp2)─H bonds of enamides without the need for metal catalyst, photocatalyst, oxidant, or light. The method can be applied to the late‐stage modification of complex molecules, synthesis of biological‐relevant oxazole analoges, and scale‐up synthesis, which all further highlight the real‐world utility of this protocol. Mechanistic studies reveal that the reaction possibly proceeds through a radical perfluoroalkylation, consecutive C─F bond heterolytic cleavage, and cyclization process. In addition, the in situ formed perfluoroalkyl radical which may also serve as an essential hydrogen abstractor.https://doi.org/10.1002/advs.2024047381,2‐difluoroalkenyl groupC─F bond functionalizationdefluorinative cyclizationfluoroalkyl halidesoxazole
spellingShingle Yu‐Lan Chen
Wei Han
Yuan‐Yuan Ren
Mengtao Ma
Danhua Ge
Zhi‐Liang Shen
Kai Guo
Xue‐Qiang Chu
Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
Advanced Science
1,2‐difluoroalkenyl group
C─F bond functionalization
defluorinative cyclization
fluoroalkyl halides
oxazole
title Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
title_full Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
title_fullStr Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
title_full_unstemmed Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
title_short Defluorinative Cyclization of Enamides with Fluoroalkyl Halides Through Two Vicinal C(sp3)─F Bonds Functionalization
title_sort defluorinative cyclization of enamides with fluoroalkyl halides through two vicinal c sp3 ─f bonds functionalization
topic 1,2‐difluoroalkenyl group
C─F bond functionalization
defluorinative cyclization
fluoroalkyl halides
oxazole
url https://doi.org/10.1002/advs.202404738
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