{"title":"用n中心自由基解锁异腈插入:光/铜协同催化合成喹唑啉酮类生物碱的一般策略","authors":"Xiaoyu Guo, Hui Wang, Zhongyan Hu*, Yu Zhao, Jinhuan Dong, Kangbao Zhong*, Yu Lan* and Xianxiu Xu*, ","doi":"10.1021/acscatal.5c0060810.1021/acscatal.5c00608","DOIUrl":null,"url":null,"abstract":"<p >Significant progress has been achieved in radical isonitrile insertion reactions, yet the reactivity of isonitriles toward <i>N</i>-centered radicals remains underexplored. Herein, we report an efficient method that enables isonitrile insertion into <i>N</i>-centered radicals, facilitated by a synergistic photocatalyst/copper catalytic system. This insertion triggers a highly efficient cascade cyclization that constitutes a flexible strategy for synthesizing alkaloids with a fused quinolizinone scaffold. Alkaloids, including luotonin A, rutaecarpine, and 2-methoxy-13-methylrutaecarpine, along with 37 natural product-like molecules, were synthesized by this method in a single step, starting from readily synthesizable <i>ortho</i>-isocyano-<i>N</i>-tosylbenzamides as <i>N</i>-radical precursors. Mechanistic investigations, encompassing photophysical, electrochemical, Einstein–Podolsky–Rosen studies, and density functional theory calculations, imply that arylisonitrile-Cu(I) complexes serve as effective reductants, quenching the excited iridium photocatalyst via single-electron transfer at the onset of the reaction. Crucially, the Cu(I)/Cu(II)/Cu(III) catalytic cycle plays a key role in sustaining the photocatalytic process and driving the radical cascade cyclization.</p>","PeriodicalId":9,"journal":{"name":"ACS Catalysis ","volume":"15 7","pages":"5307–5317 5307–5317"},"PeriodicalIF":13.1000,"publicationDate":"2025-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Unlocking Isonitrile Insertion with N-Centered Radicals: A General Synthetic Strategy toward Quinazolinone Alkaloids by Synergistic Photo/Copper Catalysis\",\"authors\":\"Xiaoyu Guo, Hui Wang, Zhongyan Hu*, Yu Zhao, Jinhuan Dong, Kangbao Zhong*, Yu Lan* and Xianxiu Xu*, \",\"doi\":\"10.1021/acscatal.5c0060810.1021/acscatal.5c00608\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >Significant progress has been achieved in radical isonitrile insertion reactions, yet the reactivity of isonitriles toward <i>N</i>-centered radicals remains underexplored. Herein, we report an efficient method that enables isonitrile insertion into <i>N</i>-centered radicals, facilitated by a synergistic photocatalyst/copper catalytic system. This insertion triggers a highly efficient cascade cyclization that constitutes a flexible strategy for synthesizing alkaloids with a fused quinolizinone scaffold. Alkaloids, including luotonin A, rutaecarpine, and 2-methoxy-13-methylrutaecarpine, along with 37 natural product-like molecules, were synthesized by this method in a single step, starting from readily synthesizable <i>ortho</i>-isocyano-<i>N</i>-tosylbenzamides as <i>N</i>-radical precursors. Mechanistic investigations, encompassing photophysical, electrochemical, Einstein–Podolsky–Rosen studies, and density functional theory calculations, imply that arylisonitrile-Cu(I) complexes serve as effective reductants, quenching the excited iridium photocatalyst via single-electron transfer at the onset of the reaction. Crucially, the Cu(I)/Cu(II)/Cu(III) catalytic cycle plays a key role in sustaining the photocatalytic process and driving the radical cascade cyclization.</p>\",\"PeriodicalId\":9,\"journal\":{\"name\":\"ACS Catalysis \",\"volume\":\"15 7\",\"pages\":\"5307–5317 5307–5317\"},\"PeriodicalIF\":13.1000,\"publicationDate\":\"2025-03-16\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"ACS Catalysis \",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acscatal.5c00608\",\"RegionNum\":1,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, PHYSICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"ACS Catalysis ","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acscatal.5c00608","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
引用次数: 0
摘要
自由基异腈插入反应已经取得了重大进展,但异腈对n中心自由基的反应性仍未得到充分研究。在此,我们报告了一种有效的方法,使异腈插入到n中心自由基,由协同光催化剂/铜催化系统促进。这种插入触发了高效的级联环化,构成了用融合喹啉酮支架合成生物碱的灵活策略。该方法以易合成的正异氰基- n -甲基苯甲酰胺为n自由基前体,一步合成了生物碱A、芦丁卡尔松和2-甲氧基-13-甲基芦丁卡尔松等生物碱及37种天然产物样分子。包括光物理、电化学、爱因斯坦-波多尔斯基-罗森研究和密度泛函理论计算在内的机理研究表明,芳基异腈- cu (I)配合物可以作为有效的还原剂,在反应开始时通过单电子转移来猝灭激发的铱光催化剂。关键是,Cu(I)/Cu(II)/Cu(III)催化循环在维持光催化过程和驱动自由基级联循环中起关键作用。
Unlocking Isonitrile Insertion with N-Centered Radicals: A General Synthetic Strategy toward Quinazolinone Alkaloids by Synergistic Photo/Copper Catalysis
Significant progress has been achieved in radical isonitrile insertion reactions, yet the reactivity of isonitriles toward N-centered radicals remains underexplored. Herein, we report an efficient method that enables isonitrile insertion into N-centered radicals, facilitated by a synergistic photocatalyst/copper catalytic system. This insertion triggers a highly efficient cascade cyclization that constitutes a flexible strategy for synthesizing alkaloids with a fused quinolizinone scaffold. Alkaloids, including luotonin A, rutaecarpine, and 2-methoxy-13-methylrutaecarpine, along with 37 natural product-like molecules, were synthesized by this method in a single step, starting from readily synthesizable ortho-isocyano-N-tosylbenzamides as N-radical precursors. Mechanistic investigations, encompassing photophysical, electrochemical, Einstein–Podolsky–Rosen studies, and density functional theory calculations, imply that arylisonitrile-Cu(I) complexes serve as effective reductants, quenching the excited iridium photocatalyst via single-electron transfer at the onset of the reaction. Crucially, the Cu(I)/Cu(II)/Cu(III) catalytic cycle plays a key role in sustaining the photocatalytic process and driving the radical cascade cyclization.
期刊介绍:
ACS Catalysis is an esteemed journal that publishes original research in the fields of heterogeneous catalysis, molecular catalysis, and biocatalysis. It offers broad coverage across diverse areas such as life sciences, organometallics and synthesis, photochemistry and electrochemistry, drug discovery and synthesis, materials science, environmental protection, polymer discovery and synthesis, and energy and fuels.
The scope of the journal is to showcase innovative work in various aspects of catalysis. This includes new reactions and novel synthetic approaches utilizing known catalysts, the discovery or modification of new catalysts, elucidation of catalytic mechanisms through cutting-edge investigations, practical enhancements of existing processes, as well as conceptual advances in the field. Contributions to ACS Catalysis can encompass both experimental and theoretical research focused on catalytic molecules, macromolecules, and materials that exhibit catalytic turnover.