Harnessing polarisation transfer to indazole and imidazole through signal amplification by reversible exchange to improve their NMR detectability.

Magnetic Resonance in Chemistry : MRC
Marianna FeketeSimon B Duckett

Abstract

The signal amplification by reversible exchange (SABRE) approach has been used to hyperpolarise the substrates indazole and imidazole in the presence of the co-ligand acetonitrile through the action of the precataysts [IrCl(COD)(IMes)] and [IrCl(COD)(SIMes)]. 2 H-labelled forms of these catalysts were also examined. Our comparison of the two precatalysts [IrCl(COD)(IMes)] and [IrCl(COD)(SIMes)], coupled with 2 H labelling of the N-heterocyclic carbene and associated relaxation and polarisation field variation studies, demonstrates the critical and collective role these parameters play in controlling the efficiency of signal amplification by reversible exchange. Ultimately, with imidazole, a 700-fold1 H signal gain per proton is produced at 400 MHz, whilst for indazole, a 90-fold increase per proton is achieved. The co-ligand acetonitrile proved to optimally exhibit a 190-fold signal gain per proton in these measurements, with the associated studies revealing the importance the substrate plays in controlling this value. Copyright © 2017 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.

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Citations

Jan 10, 2018·Angewandte Chemie·Peter J Rayner, Simon B Duckett
Dec 24, 2017·Magnetic Resonance in Chemistry : MRC·Philip NorcottSimon B Duckett
May 24, 2018·Chemistry, an Asian Journal·Kirill V KovtunovIgor V Koptyug
Jan 24, 2020·Angewandte Chemie·Kirill V KovtunovEduard Y Chekmenev
Jul 17, 2020·Chemical Communications : Chem Comm·Johannes F P ColellThomas Theis
May 22, 2018·Chemical Science·Wissam IaliSimon B Duckett
Oct 8, 2019·Chemical Science·Peter J RaynerSimon B Duckett
Jan 3, 2020·The Journal of Chemical Physics·Sara HadjialiGerd Buntkowsky
Jul 11, 2020·Catalysis Science & Technology·Ben J TicknerSimon B Duckett
Aug 13, 2020·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Ratnamala MandalChristian Hilty
Mar 20, 2021·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Nikita V ChukanovEduard Y Chekmenev
Jun 15, 2021·Magnetic Resonance in Chemistry : MRC·Keilian MacCullochThomas Theis
Jun 30, 2018·The Journal of Physical Chemistry. C, Nanomaterials and Interfaces·Roman V ShchepinEduard Y Chekmenev

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Methods Mentioned

BETA
nuclear magnetic resonance
NMR

Software Mentioned

SABRE

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