Wang Ye, Das Soumik, Aboulhosn Kareem, Champagne Sarah E, Gemmel Philipp M, Skinner Kevin C, Ragsdale Stephen W, Zimmerman Paul M, Narayan Alison R H
Life Sciences Institute, University of Michigan, Ann Arbor, Michigan 48109, United States.
Department of Chemistry, University of Michigan, Ann Arbor, Michigan 48109, United States.
J Am Chem Soc. 2024 Aug 21;146(33):23321-23329. doi: 10.1021/jacs.4c05997. Epub 2024 Aug 6.
Pyridoxal-5'-phosphate (PLP) and derivatives of this cofactor enable a plethora of reactions in both enzyme-mediated and free-in-solution transformations. With few exceptions in each category, such chemistry has predominantly involved two-electron processes. This sometimes poses a significant challenge for using PLP to build tetrasubstituted carbon centers, especially when the reaction is reversible. The ability to access radical pathways is paramount to broadening the scope of reactions catalyzed by this coenzyme. In this study, we demonstrate the ability to access a radical PLP-based intermediate and engage this radical intermediate in a number of C-C bond-forming reactions. By selection of an appropriate oxidant, single-electron oxidation of the quinonoid intermediate can be achieved, which can subsequently be applied to C-C bond-forming reactions. Through this radical reaction pathway, we synthesized a series of α-tertiary amino acids and esters to investigate the substrate scope and identify nonproductive reaction pathways. Beyond the amino acid model system, we demonstrate that other classes of amine substrates can be applied in this reaction and that a range of small molecule reagents can serve as coupling partners to the semiquinone radical. We anticipate that this versatile semiquinone radical species will be central to the development of a range of novel reactions.
磷酸吡哆醛(PLP)及其该辅因子的衍生物在酶介导的反应和溶液中的自由转化反应中能够引发大量反应。在每一类反应中,除了少数例外情况,此类化学反应主要涉及双电子过程。这有时会给利用PLP构建四取代碳中心带来重大挑战,尤其是当反应可逆时。进入自由基途径的能力对于拓宽这种辅酶催化的反应范围至关重要。在本研究中,我们展示了获得基于PLP的自由基中间体的能力,并使该自由基中间体参与许多碳-碳键形成反应。通过选择合适的氧化剂,可以实现醌型中间体的单电子氧化,随后可将其应用于碳-碳键形成反应。通过这种自由基反应途径,我们合成了一系列α-叔氨基酸和酯,以研究底物范围并确定非生产性反应途径。除了氨基酸模型体系,我们还证明了其他类别的胺底物也可应用于该反应,并且一系列小分子试剂可以作为与半醌自由基的偶联伙伴。我们预计这种多功能的半醌自由基物种将成为一系列新型反应发展的核心。