Snabilié Demi D, Ham Rens, Reek Joost N H, de Bruin Bas
Van 't Hoff Institute for Molecular Sciences, University of Amsterdam, Science Park 904, Amsterdam 1098 XH, The Netherlands.
Organometallics. 2024 May 24;43(11):1299-1307. doi: 10.1021/acs.organomet.4c00127. eCollection 2024 Jun 10.
Radical-type carbene transfer catalysis is an efficient method for the direct functionalization of C-H and C=C bonds. However, carbene radical complexes are currently formed via high-energy carbene precursors, such as diazo compounds or iodonium ylides. Many of these carbene precursors require additional synthetic steps, have an explosive nature, or generate halogenated waste. Consequently, the utilization of carbene radical catalysis is limited by specific carbene precursors that access the carbene radical intermediate. In this study, we generate a cobalt(III) carbene radical complex from dimethyl malonate, which is commercially available and bench-stable. EPR and NMR spectroscopy were used to identify the intermediates and showed that the cobalt(III) carbene radical complex is formed upon light irradiation. In the presence of styrene, carbene transfer occurred, forming cyclopropane as the product. With this photochemical method, we demonstrate that dimethyl malonate can be used as an alternative carbene precursor in the formation of a cobalt(III) carbene radical complex.
自由基型卡宾转移催化是一种用于C-H键和C=C键直接官能团化的有效方法。然而,目前卡宾自由基配合物是通过高能卡宾前体形成的,如重氮化合物或碘鎓叶立德。这些卡宾前体中的许多需要额外的合成步骤,具有爆炸性,或产生卤化废物。因此,卡宾自由基催化的应用受到能够生成卡宾自由基中间体的特定卡宾前体的限制。在本研究中,我们从丙二酸二甲酯生成了钴(III)卡宾自由基配合物,丙二酸二甲酯是市售的且在实验室条件下稳定。电子顺磁共振光谱和核磁共振光谱被用于鉴定中间体,并表明钴(III)卡宾自由基配合物在光照下形成。在苯乙烯存在的情况下,发生了卡宾转移,形成环丙烷作为产物。通过这种光化学方法,我们证明了丙二酸二甲酯可以用作形成钴(III)卡宾自由基配合物的替代卡宾前体。