Monitoring hydrogenation reactions using benchtop 2D NMR with extraordinary sensitivity and spectral resolution
|Author:||Gołowicz, Dariusz1,2; Kazimierczuk, Krzysztof2; Urbańczyk, Mateusz2,3;|
1Faculty of Chemistry, Biological and Chemical Research Centre, University of Warsaw, Żwirki i Wigury 101, 02-089 Warsaw (Poland)
2Centre of New Technologies, University of Warsaw, Banacha 2 C, 02-097 Warsaw (Poland)
3NMR Research Unit, University of Oulu, 90014 Oulu (Finland)
4Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland)
|Online Access:||PDF Full Text (PDF, 1.5 MB)|
|Persistent link:|| http://urn.fi/urn:nbn:fi-fe201903067329
John Wiley & Sons,
|Publish Date:|| 2019-03-06
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.
|Pages:||196 - 200|
|Type of Publication:||
A1 Journal article – refereed
|Field of Science:||
114 Physical sciences
116 Chemical sciences
The authors would like to thank the National Science Centre of Poland for support us with the grants OPUS 11 (2016/21/B/ST4/02162) and OPUS 9 (2015/17/B/ST4/04221). MU acknowledges financial support from the Kvantum Institute (University of Oulu).
© 2019 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA. This is an open access article under the terms of the Creative Commons Attribution‐NonCommercial License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited and is not used for commercial purposes.