N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, Leninsky prosp. 47, Moscow, 119991, Russia.
A. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Vavilov str. 28, Moscow, 119991, Russia.
Org Biomol Chem. 2020 Feb 19;18(7):1436-1448. doi: 10.1039/c9ob02668a.
An efficient route to pyrazolo[1,5-a]pyridines by Cu(OAc)2-promoted oxidative [3 + 2]-annulation of nitroalkenes with in situ generated pyridinium imines is developed. The reaction with α-fluoronitroalkenes enables the first preparative synthesis of 3-fluoro-pyrazolo[1,5-a]pyridines. Cycloaddition with α-unsubstituted nitroalkenes provides access to 3-nitro-pyrazolo[1,5-a]pyridines in excellent yields. A broad transformation scope was demonstrated. Both electron-rich and electron-deficient nitroalkenes as well as different aminopyridinium salts can be used for the assembly of the target pyrazolo[1,5-a]pyridines. The related aza-heterocycles, namely, pyrazolo[1,5-a]pyrazines and pyrazolo[1,5-b]pyridazines, were successfully prepared via the present methodology. The possible mechanism of the reaction is discussed.
一种通过 Cu(OAc)2 促进的硝基亚乙烯与原位生成的吡啶亚胺的高效氧化 [3 + 2]-环化反应,来合成吡唑并[1,5-a]吡啶的方法被开发出来。与α-氟代硝基亚乙烯的反应实现了 3-氟代吡唑并[1,5-a]吡啶的首次制备性合成。与α-未取代的硝基亚乙烯的环加成以优异的收率提供了 3-硝基吡唑并[1,5-a]吡啶。该方法展示了广泛的转化范围。富电子和缺电子的硝基亚乙烯以及不同的氨基吡啶𬭩盐都可以用于目标吡唑并[1,5-a]吡啶的组装。通过本方法还成功制备了相关的氮杂杂环,即吡唑并[1,5-a]吡嗪和吡唑并[1,5-b]哒嗪。讨论了反应的可能机制。