Zheng Long, Li Ying-Chao, Wu Yichen, Wang Peng
State Key Laboratory of Organometallic Chemistry and Shanghai-Hong Kong Joint Laboratory in Chemical Synthesis, Shanghai Institute of Organic Chemistry, University of Chinese Academy of Sciences, CAS, 345 Lingling Road, Shanghai, 200032, P. R. China.
School of Chemistry and Materials Science, Hangzhou Institute for Advanced Study, University of Chinese Academy of Sciences, 1 Sub-lane Xiangshan, Hangzhou, 310024, P. R. China.
Adv Sci (Weinh). 2024 Dec;11(45):e2409457. doi: 10.1002/advs.202409457. Epub 2024 Oct 14.
The transition metal-catalyzed direct coupling reactions involving electron-rich Fischer carbene species are largely underdeveloped and remain a big challenge. Here, a direct coupling reaction of azoles and azine N-oxides is reported with Fischer copper carbene species bearing an α-siloxy group i, which can be in situ generated from acylsilanes catalytically under photoirradiation and redox-neutral conditions. This coupling reaction between electron-rich α-siloxy Fischer Cu-carbene species with hard carbanion nucleophiles may undergo a bimetallic relay process, which is confirmed by the kinetic analysis and in situ NMR analysis. This reaction features mild conditions and remarkable heterocycle compatibility. Notably, this protocol tolerates a series of azole or azine N-oxide derivatives, including benzoxazole, benzothiazole, benzoimidazole, benzoisoxazole, oxazole, oxadiazole, triazolo[4,3-a]pyridine, purine, caffeine, pyridine N-oxide, quinoline N-oxide, pyrazine N-oxide, pyridazine N-oxide, etc. The synthetic value of this approach is demonstrated by the efficient synthesis of a histamine h4 receptor ligand and a marketed drug carbinoxamine.
涉及富电子费歇尔卡宾物种的过渡金属催化直接偶联反应在很大程度上尚未得到充分发展,仍然是一个巨大的挑战。在此,报道了唑类和嗪N-氧化物与带有α-硅氧基i的费歇尔铜卡宾物种的直接偶联反应,该物种可在光照射和氧化还原中性条件下由酰基硅烷催化原位生成。富电子的α-硅氧基费歇尔铜卡宾物种与硬碳负离子亲核试剂之间的这种偶联反应可能经历双金属接力过程,这通过动力学分析和原位核磁共振分析得到证实。该反应具有温和的条件和显著的杂环兼容性。值得注意的是,该方法适用于一系列唑类或嗪N-氧化物衍生物,包括苯并恶唑、苯并噻唑、苯并咪唑、苯并异恶唑、恶唑、恶二唑、三唑并[4,3-a]吡啶、嘌呤、咖啡因、吡啶N-氧化物、喹啉N-氧化物、吡嗪N-氧化物、哒嗪N-氧化物等。通过高效合成组胺H4受体配体和市售药物卡比沙明证明了该方法的合成价值。