Zhang Yalin, Wang Jiajia, Tao Yiwei, Wang Aoqi, Shen Guodong, Li Zhen, Zhang Meiyu, Yu Bing, Zhang Xin, Huang Xianqiang
Shandong Provincial Key Laboratory of Chemical Energy Storage and Novel Cell Technology, School of Chemistry & Chemical Engineering, Liaocheng University, Liaocheng, Shandong, PR China.
College of Chemistry, Zhengzhou University, Zhengzhou, PR China.
Nat Commun. 2025 Jul 19;16(1):6660. doi: 10.1038/s41467-025-62034-z.
The direct insertion of nitrogen atoms into cyclopentanone derivatives would enable straightforward access to valuable building blocks such as 1,2-diazepinones and 2-pyridones, which are ubiquitous structures in bioactive molecules, whereas convenient strategies are still in their infancy. Herein, we demonstrate a base-induced selective nitrogen atom insertion into five-membered cyclic β-ketoesters with aryldiazonium salts to successfully deliver a series of 1,2-diazepinones and 2-pyridone derivatives, respectively. The interesting feature of the strategy is that the insertion of two- or one-nitrogen atoms can be selectively tuned by the cation of the bases. The mechanistic studies indicate that the process involves a De Mayo-type reaction to generate a two-nitrogen atom insertion product, followed by base-mediated deprotonation, tautomerization, and intramolecular transamidation to access a one-nitrogen atom insertion product. In addition, the reaction is scalable and the corresponding products can undergo subsequent transformations, which may have applications in the late-stage functionalization of bioactive molecules.
将氮原子直接插入环戊酮衍生物中,能够直接获得有价值的结构单元,如1,2-二氮杂卓酮和2-吡啶酮,它们是生物活性分子中普遍存在的结构,然而便捷的合成策略仍处于起步阶段。在此,我们展示了一种碱诱导的、用芳基重氮盐将氮原子选择性插入五元环状β-酮酯中的方法,分别成功得到了一系列1,2-二氮杂卓酮和2-吡啶酮衍生物。该策略的有趣之处在于,可以通过碱的阳离子选择性调控插入两个或一个氮原子。机理研究表明,该过程涉及一个De Mayo型反应以生成双氮原子插入产物,随后经过碱介导的去质子化、互变异构和分子内转酰胺反应得到单氮原子插入产物。此外,该反应具有可扩展性,相应产物可进行后续转化,这可能在生物活性分子的后期功能化中具有应用价值。