Suppr超能文献

通过对映选择性霍夫曼-勒夫勒-弗赖塔格反应合成手性吡咯烷。

Chiral pyrrolidines via an enantioselective Hofmann-Löffler-Freytag reaction.

作者信息

Laohapaisan Pavitra, Roy Ipshita, Nagib David A

机构信息

Department of Chemistry and Biochemistry, The Ohio State University, Columbus, OH 43210.

出版信息

Chem Catal. 2024 Dec 19;4(12). doi: 10.1016/j.checat.2024.101149. Epub 2024 Oct 16.

Abstract

Radical C-H aminations enable rapid access to the most common heterocycles in medicines (e.g. pyrrolidines), yet stereocontrol of these powerful transformations remains a challenge. Here, we report the discovery of the first enantio- and regio- selective C-H imination, which readily converts ketones to enantioenriched pyrrolidines. This enantioselective Hofmann-Löffler-Freytag reaction mechanism entails iminyl radical generation from an oxime by a chiral Cu catalyst that facilitates 1,5-H-atom transfer (HAT) to form a remote C-radical, regioselectively. The selective capture of this alkyl radical as an organocopper(III) complex then mediates highly stereoselective reductive elimination to unprotected pyrrolines. The broad steric and electronic scope of this remote C-H amination has been probed systematically, along with key mechanistic aspects of enantiodetermination, radical intermediacy, and atypical Cu(III) ligands that enable this uniquely selective C-N coupling. Importantly, either (1) reductions or (2) nucleophilic additions to these enantioenriched pyrrolines provide the most rapid syntheses of chiral pyrrolidines to date.

摘要

自由基C-H胺化反应能够快速构建药物中最常见的杂环(如吡咯烷),然而,对这些强大转化反应的立体控制仍然是一个挑战。在此,我们报告了首例对映和区域选择性C-H亚胺化反应的发现,该反应可将酮轻松转化为对映体富集的吡咯烷。这种对映选择性霍夫曼-勒夫勒-弗赖塔格反应机制涉及通过手性铜催化剂从肟生成亚胺基自由基,该催化剂促进1,5-氢原子转移(HAT)以区域选择性地形成远程C-自由基。然后,将该烷基自由基选择性捕获为有机铜(III)配合物,介导高度立体选择性的还原消除反应生成未受保护的吡咯啉。我们系统地探究了这种远程C-H胺化反应广泛的空间和电子范围,以及对映体决定、自由基中间体和实现这种独特选择性C-N偶联的非典型铜(III)配体的关键机理。重要的是,(1)对这些对映体富集的吡咯啉进行还原或(2)亲核加成,均可实现迄今为止最快的手性吡咯烷合成。

相似文献

10
Copper-Catalyzed Radical Relay for Asymmetric Radical Transformations.铜催化的自由基接力用于不对称自由基转化
Acc Chem Res. 2018 Sep 18;51(9):2036-2046. doi: 10.1021/acs.accounts.8b00265. Epub 2018 Sep 5.

引用本文的文献

1
Enantioselective Borylcupration/Cyclization of Alkene-Tethered Oxime Esters.烯烃连接的肟酯的对映选择性硼氢化铜化/环化反应
Angew Chem Int Ed Engl. 2025 Mar 3;64(10):e202420479. doi: 10.1002/anie.202420479. Epub 2025 Feb 11.

本文引用的文献

7
Asymmetric Syntheses of Enantioenriched 2,5-Disubstituted Pyrrolidines.对映体富集的2,5-二取代吡咯烷的不对称合成。
ACS Org Inorg Au. 2023 Mar 8;3(3):120-129. doi: 10.1021/acsorginorgau.2c00061. eCollection 2023 Jun 7.
9
Nitrene transfer catalysts for enantioselective C-N bond formation.用于对映选择性C-N键形成的氮宾转移催化剂。
Nat Rev Chem. 2021 Aug;5(8):580-594. doi: 10.1038/s41570-021-00291-4. Epub 2021 Jun 28.

文献AI研究员

20分钟写一篇综述,助力文献阅读效率提升50倍。

立即体验

用中文搜PubMed

大模型驱动的PubMed中文搜索引擎

马上搜索

文档翻译

学术文献翻译模型,支持多种主流文档格式。

立即体验