Department of Chemistry and ZJU-NHU United R&D Center, Zhejiang University, 38 Zheda Road, Hangzhou, 310027, P. R. China.
State Key Laboratory of Chemical Engineering and College of Chemical and Biological Engineering, Zhejiang University, 38 Zheda Road, Hangzhou, 310027, P. R. China.
Angew Chem Int Ed Engl. 2021 Mar 15;60(12):6631-6638. doi: 10.1002/anie.202014478. Epub 2021 Feb 3.
The critical role of double hydrogen bonds was addressed for the aerobic α-hydroxylation of ketones catalyzed by 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD), in the absence of either a metal catalyst or phosphine reductant. Experimental and theoretical investigations were performed to study the mechanism. In addition to initiating the reaction by proton abstraction, a more important role of TBD was revealed, that is, to enhance the oxidizing ability of peroxide intermediates, allowing DMSO to be used rather than commonly used phosphine reductants. Further characterizations with nuclear Overhauser effect spectroscopy (NOESY) confirmed the presence of double hydrogen bonds between TBD and the ketone, and kinetic studies suggested the attack of dioxygen on the TBD-enol adduct to be the rate-determining step. This work should encourage the application of TBD as a catalyst for oxidations.
双氢键在 1,5,7-三氮杂二环[4.4.0]癸-5-烯(TBD)催化的酮的需氧α-羟化中起着至关重要的作用,在此过程中既不需要金属催化剂也不需要膦还原剂。进行了实验和理论研究来探究其反应机理。除了通过质子抽提引发反应之外,还揭示了 TBD 的一个更重要的作用,即增强过氧化物中间体的氧化能力,从而可以使用 DMSO 而不是常用的膦还原剂。利用核 Overhauser 效应光谱(NOESY)进一步进行的特征分析证实了 TBD 和酮之间存在双氢键,动力学研究表明,氧气进攻 TBD-烯醇加合物是速率决定步骤。这项工作应该会鼓励将 TBD 用作氧化反应的催化剂。