Horsewill Samuel J, Sharrock Katherine M M, Fehér Péter P, Woolley Jack M, Pápai Imre, Scott Daniel J
Department of Chemistry, University of Bath, Claverton Down, Bath, BA2 7AY, UK.
Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK.
Angew Chem Int Ed Engl. 2025 Aug 18;64(34):e202506701. doi: 10.1002/anie.202506701. Epub 2025 Jul 2.
Photoredox chemistry has seen a dramatic rise in popularity in recent years, but mechanistic understanding has persistently lagged behind reaction development itself. This is particularly true for the emerging area of consecutive photoinduced electron transfer (conPET), which has attracted both great interest due to its ability to activate inert substrates selectively and under mild conditions and continuing controversy over its mechanistic feasibility. We describe herein the isolation of the key radical intermediate state of an acridinium-based conPET catalyst and detailed investigations of its photochemistry by a suite of (photo)reactivity, photoluminescence and transient absorption techniques, supported by computational studies. We observe strong wavelength and solvent dependencies in the reactivity profile, which correlate well with observations of a long-lived, fluorescent excited state that would be compatible with diffusion-limited reactivity. However, photoluminescence and transient absorption spectroscopies suggest that, counter-intuitively, this state does not actually participate in reactivity. Instead, changes occur far faster than the diffusion limit, which provides strong, direct evidence for preassembly of the photocatalyst and substrate prior to photoexcitation. Further inspection also indicates parallel formation of solvated electrons, likely providing the major pathway under previously reported synthetic conditions, suggesting that otherwise competing rationales for conPET can in fact operate simultaneously.
近年来,光氧化还原化学的受欢迎程度急剧上升,但对其机理的理解一直落后于反应开发本身。对于新兴的连续光诱导电子转移(conPET)领域来说尤其如此,该领域因其能够在温和条件下选择性地活化惰性底物而备受关注,同时其机理的可行性也一直存在争议。我们在此描述了一种基于吖啶鎓的conPET催化剂关键自由基中间体状态的分离,并通过一系列(光)反应性、光致发光和瞬态吸收技术对其光化学进行了详细研究,同时辅以计算研究。我们观察到反应性分布中存在强烈的波长和溶剂依赖性,这与对一种与扩散限制反应性相容的长寿命荧光激发态的观察结果高度相关。然而,光致发光和瞬态吸收光谱表明,与直觉相反,这种状态实际上并不参与反应。相反,变化发生的速度远远快于扩散极限,这为光催化剂和底物在光激发之前的预组装提供了有力的直接证据。进一步的研究还表明溶剂化电子会同时形成,这可能是先前报道的合成条件下的主要途径,这表明conPET中其他相互竞争的原理实际上可以同时起作用。