Merging Gradient-Based Methods to Improve Benchtop NMR Spectroscopy: A New Tool for Flow Reaction Optimization
| Autor: | François-Xavier Felpin, Shrikant Kunjir, Vincent Coeffard, Mireia Rodriguez-Zubiri, Patrick Giraudeau, Jonathan Farjon |
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| Přispěvatelé: | Chimie Et Interdisciplinarité : Synthèse, Analyse, Modélisation (CEISAM), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Université de Nantes - Faculté des Sciences et des Techniques, Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS) |
| Rok vydání: | 2020 |
| Předmět: |
Materials science
Spectrometer Resolution (electron density) Context (language use) Pulse sequence 02 engineering and technology Nuclear magnetic resonance spectroscopy Flow chemistry 010402 general chemistry 021001 nanoscience & nanotechnology 01 natural sciences Atomic and Molecular Physics and Optics 0104 chemical sciences [CHIM]Chemical Sciences Sensitivity (control systems) Physical and Theoretical Chemistry Spectral resolution 0210 nano-technology Biological system ComputingMilieux_MISCELLANEOUS |
| Zdroj: | HAL ChemPhysChem ChemPhysChem, Wiley-VCH Verlag, 2020 ChemPhysChem, Wiley-VCH Verlag, 2020, 21 (20), pp.2311-2319. ⟨10.1002/cphc.202000573⟩ |
| ISSN: | 1439-7641 1439-4235 |
| DOI: | 10.1002/cphc.202000573⟩ |
| Popis: | International audience; Emerging low cost, compact NMR spectrometers that can be connected in-line to a flow reactor are suited to study reaction mixtures. The main limitation of such spectrometers arises from their lower magnetic field inducing a reduced sensitivity and a weaker spectral resolution. For enhancing the spectral resolution, the merging of Pure-Shift methods recognized for line narrowing with solvent elimination schemes was implemented in the context of mixtures containing protonated solvents. One more step was achieved to further enhance the resolution power on compact systems, thanks to multiple elimination schemes prior to Pure-Shift pulse sequence elements. For the first time, we were able to remove up to 6 protonated solvent signals simultaneously by dividing their intensity by 500 to 1700 with a concomitant spectral resolution enhancement for signals of interest from 9 to 12 as compared to the standard 1D 1 H. Then, the potential of this new approach was shown on the flow synthesis of a complex benzoxanthenone structure. |
| Databáze: | OpenAIRE |
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