Real-time reaction monitoring by ultrafast 2D NMR on a benchtop spectrometer.
Reaction monitoring is widely used to follow chemical processes in a broad range of application fields. Recently, the development of robust benchtop NMR spectrometers has brought NMR under the fume hood, making it possible to monitor chemical reactions in a safe and accessible environment. However, these low-field NMR approaches suffer from limited resolution leading to strong peak overlaps, which can limit their application range. Here, we propose an approach capable of recording ultrafast 2D NMR spectra on a compact spectrometer and of following in real time reactions in the synthetic chemistry laboratory. This approach--whose potential is shown here on a Heck-Matsuda reaction--is highly versatile; the duration of the measurement can be optimized to follow reactions whose time scale ranges from between a few tens of seconds to a few hours. It makes it possible to monitor complex reactions in non-deuterated solvents, and to confirm in real time the molecular structure of the compounds involved in the reaction while giving access to relevant kinetic parameters.
CEISAM CNRS, UMR6230, Université de Nantes, BP 92208, 2 rue de la Houssinière, 44322 Nantes, France. patrick.giraudeau@univ-nantes.fr.
Boris
B
Gouilleux
Benoît
B
Charrier
Ernesto
E
Danieli
Jean-Nicolas
JN
Dumez
Serge
S
Akoka
François-Xavier
FX
Felpin
Mireia
M
Rodriguez-Zubiri
Patrick
P
Giraudeau
D002384:Catalysis; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation*; D009682:Magnetic Resonance Spectroscopy; D015394:Molecular Structure; D010165:Palladium / Q000737:chemistry; D013997:Time Factors
D010165:Palladium