波谱学杂志 ›› 2008, Vol. 25 ›› Issue (4): 461-469.

• 研究论文 • 上一篇    下一篇

钯催化Csp-Csp3偶联反应的13C NMR定量研究

李芳1,3;赵应声2;雷爱文2;刘买利1*   

  1. [1. 波谱与原子分子物理国家重点实验室(中国科学院 武汉物理与数学研究所), 湖北 武汉 430071; 2. 武汉大学 化学与分子科学学院,湖北 武汉 430072; 3. 中国科学院 研究生院, 北京 100049]
  • 收稿日期:2008-06-02 修回日期:2008-06-08 出版日期:2008-12-05 发布日期:2009-12-05
  • 通讯作者: 刘买利

Palladium Catalyzed Csp-Csp3 Bond Formation Reaction Studied by 13C NMR

LI Fang1,3;ZHAO Ying-sheng2;LEI Ai-wen2;LIU Mai-li1*   

  1. [1.State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, (Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences), Wuhan 430071, China; 2.College of Chemistry and Molecular Science, Wuhan University, Wuhan, 430072, China; 3.Graduate School of Chinese Academy of Sciences, Beijing 100049, China]
  • Received:2008-06-02 Revised:2008-06-08 Online:2008-12-05 Published:2009-12-05
  • Contact: LIU Mai-li

摘要: 利用NOE(Nuclear Overhauser Effect)增强的13C NMR方法对钯催化Csp-Csp3偶联反应过程进行实时、定量监测. 通过制作浓度曲线的方法定量分析了反应过程中各组分的浓度变化. 实验表明,同一物质各个共振峰的NOE增强倍数基本不变. 结果证实了几个主要反应物和产物的含量变化之间具有相关性,提示这些物质同属一个反应过程,为早期提出的反应机理(Zhao Y S, et al. J Am Chem Soc, 2006, 128: 15 048-15 049)提供了实验证据. 说明13C NMR能准确地提供反应体系中各物质的浓度变化信息,是化学反应机理的有效研究手段.

关键词: 13C NMR, 钯催化Csp-Csp3偶联反应, 反应机理, 实时, 定量

Abstract: NOE-enhanced 13C NMR spectroscopy was used to study palladium-catalyzed Csp-Csp3 bond formation reaction in real-time. The NOE factors for different peaks of the same substance were found to be almost the same throughout the course of reaction. The changes of the concentrations of the reactants and products were measured quantitatively during the reaction. The results of the NMR experiments provided direct evidence for the reaction mechanism proposed by Lei et al (J Am Chem Soc, 2006, 128: 15 048-15 049).

Key words: 13C NMR, palladium-catalyzed Csp-Csp3 bond formation reaction, reaction mechanism, real time, quantitatively

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