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Gołowicz D, Kazimierczuk K, Urbańczyk M, et al. Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution. ChemistryOpen. 2019;8(2):196-200doi: 10.1002/open.201800294.
Gołowicz, D., Kazimierczuk, K., Urbańczyk, M., & Ratajczyk, T. (2019). Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution. ChemistryOpen, 8(2), 196-200. https://doi.org/10.1002/open.201800294
Gołowicz, Dariusz, et al. "Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution." ChemistryOpen vol. 8,2 (2019): 196-200. doi: https://doi.org/10.1002/open.201800294
Gołowicz D, Kazimierczuk K, Urbańczyk M, Ratajczyk T. Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution. ChemistryOpen. 2019 Feb 14;8(2):196-200. doi: 10.1002/open.201800294. eCollection 2019 Feb. PMID: 30815327; PMCID: PMC6376214.
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ChemistryOpen. 2019 Feb 14;8(2):196-200. doi: 10.1002/open.201800294. eCollection 2019 Feb.

Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution.

ChemistryOpen

Dariusz Gołowicz, Krzysztof Kazimierczuk, Mateusz Urbańczyk, Tomasz Ratajczyk

Affiliations

  1. Faculty of Chemistry, Biological and Chemical Research Centre University of Warsaw ?wirki i Wigury 101 02-089 Warsaw Poland.
  2. Centre of New Technologies University of Warsaw Banacha 2?C 02-097 Warsaw Poland.
  3. NMR Research Unit University of Oulu 90014 Oulu Finland.
  4. Institute of Physical Chemistry Polish Academy of Sciences Kasprzaka 44/52 01-224 Warsaw Poland.

PMID: 30815327 PMCID: PMC6376214 DOI: 10.1002/open.201800294

Abstract

Low-field benchtop nuclear magnetic resonance (BT-NMR) spectrometers with Halbach magnets are being increasingly used in science and industry as cost-efficient tools for the monitoring of chemical reactions, including hydrogenation. However, their use of low-field magnets limits both resolution and sensitivity. In this paper, we show that it is possible to alleviate these two problems through the combination of parahydrogen-induced polarization (PHIP) and fast correlation spectroscopy with time-resolved non-uniform sampling (TR-NUS). PHIP can enhance NMR signals so that substrates are easily detectable on BT-NMR spectrometers. The interleaved acquisition of one- and two-dimensional spectra with TR-NUS provides unique insight into the consecutive moments of hydrogenation reactions, with a spectral resolution unachievable in a standard approach. We illustrate the potential of the technique with two examples: the hydrogenation of ethylphenyl propiolate and the hydrogenation of a mixture of two substrates - ethylphenyl propiolate and ethyl 2-butynoate.

Keywords: benchtop NMR; non-uniform sampling; parahydrogen-induced polarization; reaction monitoring

Conflict of interest statement

The authors declare no conflict of interest.

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