Laohapaisan Pavitra, Roy Ipshita, Nagib David A
Department of Chemistry and Biochemistry, The Ohio State University, Columbus, OH 43210.
Chem Catal. 2024 Dec 19;4(12). doi: 10.1016/j.checat.2024.101149. Epub 2024 Oct 16.
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.
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。