[4+1] Heteroannulation to Form 1‐Pyrrolines through Alder‐Ene Reaction of in situ Generated Ynimines: Development and Application in Total Synthesis of Borrecapine

We report in this paper a novel Cu-catalyzed synthesis of polysubstituted 1-pyrrolines. The reaction of β,γ-unsaturated oxime esters 4 with terminal alkynes 5 in the presence of a catalytic amount of Cu(OAc)<sub>2</sub> and 2,2'-biquinoline affords the corresponding 1,6-enynimines, which undergo a highly stereoselective Alder-ene reaction to afford 1-pyrrolines with concomitant generation of a quaternary carbon and a 2-azadiene motif. It represents an unusual [4+1] heteroannulation reaction wherein terminal alkynes act as a one carbon donor and are 1,1-difunctionalized. Mechanistic studies suggest that the allylic hydrogen trans to the oxime ester main chain is selectively transferred to the electron-rich alkyne during the pericyclic reaction. The resulting 1-pyrrolines undergo facile acid-catalyzed regioselective Wagner-Meerwein rearrangement to provide 2H-pyrroles in excellent yields. The 2H-pyrroles are also accessible from 4 and 5 in a one-pot manner without isolation of the 1-pyrrolines. Leveraging this heteroannulation reaction as a key step, the first total synthesis of borrecapine, a 2,3,3,5-tetrasubstituted pyrrolidine, is accomplished.

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Publication Details

Journal
Angewandte Chemie International Edition
Published
2024-08-16
DOI
https://doi.org/10.1002/anie.202414612
Citations
9
Primary Topic
Asymmetric Synthesis and Catalysis
Type
article
Field-Weighted Citation Impact
2.25

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article

[4+1] Heteroannulation to Form 1‐Pyrrolines through Alder‐Ene Reaction of in situ Generated Ynimines: Development and Application in Total Synthesis of Borrecapine

Rémi Lavernhe, Jieping Zhu, Qian Wang
9 citations
Angewandte Chemie International Edition
Asymmetric Synthesis and Catalysis
2.25
article

[4+1] Heteroannulation to Form 1‐Pyrrolines through Alder‐Ene Reaction of in situ Generated Ynimines: Development and Application in Total Synthesis of Borrecapine

Rémi Lavernhe, Jieping Zhu, Qian Wang
article en
9 citations

Abstract

We report in this paper a novel Cu-catalyzed synthesis of polysubstituted 1-pyrrolines. The reaction of β,γ-unsaturated oxime esters 4 with terminal alkynes 5 in the presence of a catalytic amount of Cu(OAc)<sub>2</sub> and 2,2'-biquinoline affords the corresponding 1,6-enynimines, which undergo a highly stereoselective Alder-ene reaction to afford 1-pyrrolines with concomitant generation of a quaternary carbon and a 2-azadiene motif. It represents an unusual [4+1] heteroannulation reaction wherein terminal alkynes act as a one carbon donor and are 1,1-difunctionalized. Mechanistic studies suggest that the allylic hydrogen trans to the oxime ester main chain is selectively transferred to the electron-rich alkyne during the pericyclic reaction. The resulting 1-pyrrolines undergo facile acid-catalyzed regioselective Wagner-Meerwein rearrangement to provide 2H-pyrroles in excellent yields. The 2H-pyrroles are also accessible from 4 and 5 in a one-pot manner without isolation of the 1-pyrrolines. Leveraging this heteroannulation reaction as a key step, the first total synthesis of borrecapine, a 2,3,3,5-tetrasubstituted pyrrolidine, is accomplished.

Angewandte Chemie International EditionVol. 64(2)
École Polytechnique Fédérale de Lausanne (CH)
National Science Foundation, École Polytechnique Fédérale de Lausanne, Schweizerischer Nationalfonds zur Förderung der Wissenschaftlichen Forschung
Clean water and sanitation
Openalex Percentile: Top 12%
Asymmetric Synthesis and Catalysis
2.25
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