Li Mochen, Zhang Tiexin, Shi Yusheng, He Cheng, Duan Chunying
State Key Laboratory of Fine Chemicals, Frontier Science Center for Smart Materials, School of Chemical Engineering, School of Chemistry, Dalian University of Technology, Dalian, 116024, P. R. China.
State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing, 210023, P. R. China.
Angew Chem Int Ed Engl. 2024 Aug 19;63(34):e202406161. doi: 10.1002/anie.202406161. Epub 2024 Jul 22.
Proton-coupled electron transfer (PCET) imparts an energetic advantage over single electron transfer in activating inert substances. Natural PCET enzyme catalysis generally requires tripartite preorganization of proton relay, substrate-bound active center, and redox mediator, making the processes efficient and precluding side reactions. Inspired by this, a heterogeneous photocatalytic PCET system was established to achieve higher PCET driving forces by modifying proton relays into anthraquinone-based anionic coordination polymers. The proximally separated proton relays and photoredox-mediating anthraquinone moiety allowed pre-assembly of inert substrate between them, merging proton and electron into unsaturated bonds by photoreductive PCET, which enhanced reaction kinetics compared with the counter catalyst without proton relay. This photocatalytic PCET method was applied to a broad-scoped reduction of aryl ketones, unsaturated carbonyls, and aromatic compounds. The distinctive regioselectivities for the reduction of isoquinoline derivatives were found to occur on the carbon-ring sides. PCET-generated radical intermediate of quinoline could be trapped by alkene for proton relay-assisted Minisci addition, forming the pharmaceutical aza-acenaphthene scaffold within one step. When using heteroatom(X)-H/C-H compounds as proton-electron donors, this protocol could activate these inert bonds through photooxidative PCET to afford radicals and trap them by electron-deficient unsaturated compounds, furnishing the direct X-H/C-H functionalization.
质子耦合电子转移(PCET)在活化惰性物质方面比单电子转移具有能量优势。天然PCET酶催化通常需要质子中继、底物结合活性中心和氧化还原介质的三方预组织,从而使过程高效并排除副反应。受此启发,建立了一种多相光催化PCET系统,通过将质子中继修饰为基于蒽醌的阴离子配位聚合物来实现更高的PCET驱动力。近端分离的质子中继和光氧化还原介导的蒽醌部分允许惰性底物在它们之间进行预组装,通过光还原PCET将质子和电子合并到不饱和键中,与没有质子中继的反催化剂相比,这增强了反应动力学。这种光催化PCET方法被应用于芳基酮、不饱和羰基化合物和芳香族化合物的广泛还原。发现异喹啉衍生物还原的独特区域选择性发生在碳环侧。喹啉的PCET生成的自由基中间体可以被烯烃捕获,用于质子中继辅助的Minisci加成,一步形成药物氮杂苊支架。当使用杂原子(X)-H/C-H化合物作为质子-电子供体时,该方案可以通过光氧化PCET活化这些惰性键以提供自由基,并通过缺电子不饱和化合物捕获它们,实现直接的X-H/C-H官能化。