Abstract: NOE-enhanced ¹³C NMR spectroscopy was used to study palladium-catalyzed C_sp-C_sp3 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 C_sp-C_sp3 bond formation reaction, reaction mechanism, real time, quantitatively