Kuribara Takahito, Kaneki Ayahito, Matsuda Yu, Nemoto Tetsuhiro
Institute for Advanced Academic Research, Chiba University, 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522, Japan.
Graduate School of Pharmaceutical Sciences, Chiba University, 1-8-1, Inohana, Chuo-ku, Chiba 260-8675, Japan.
J Am Chem Soc. 2024 Jul 31;146(30):20904-20912. doi: 10.1021/jacs.4c05414. Epub 2024 Jul 20.
Although divalent Sm reagents are some of the most important single-electron transfer reagents for reductive transformations, their catalytic applications are challenging. In this study, a bidentate phosphine oxide ligand substituted with 9,10-diphenylanthracene as a visible-light antenna was designed for Sm-catalyzed reduction reactions under mild reaction conditions. Pinacol coupling of aryl ketones and aldehydes was developed with 1 mol % of Sm catalyst and organic amine (DIPEA) as a sacrificial mild reductant. Mechanistic studies suggest that the visible-light-antenna ligand coordinates to Sm(III) and reduces Sm(III) to Sm(II) under visible-light irradiation. The catalytic system is also applicable for cross-pinacol coupling and other single-electron reductive transformations, including aza-pinacol coupling, flavone dimerization, C-O bond cleavage, C-C ring-opening of cyclopropane, ketyl-olefin coupling, and cross-coupling of the ketyl radical with the α-amino radical.
尽管二价钐试剂是用于还原转化的一些最重要的单电子转移试剂,但其催化应用具有挑战性。在本研究中,设计了一种用9,10-二苯基蒽作为可见光天线取代的双齿氧化膦配体,用于在温和反应条件下的钐催化还原反应。芳基酮和醛的频哪醇偶联反应是用1 mol%的钐催化剂和有机胺(DIPEA)作为牺牲性温和还原剂进行的。机理研究表明,可见光天线配体与Sm(III)配位,并在可见光照射下将Sm(III)还原为Sm(II)。该催化体系还适用于交叉频哪醇偶联和其他单电子还原转化反应,包括氮杂频哪醇偶联、黄酮二聚化、C-O键裂解、环丙烷的C-C开环、酮基-烯烃偶联以及酮基自由基与α-氨基自由基的交叉偶联反应。