Ultraselective, Ultrahigh Resolution 1D TOCSY

Author:

Montgomery James R. D.12ORCID,Gates Emma L.1ORCID,Smith Marshall J.13ORCID,Taylor Daniel A.14ORCID,Bradley Jonathan P.5ORCID,Berry Daniel B. G.5ORCID,Kiraly Peter16ORCID,Nilsson Mathias1ORCID,Morris Gareth A.1ORCID,Adams Ralph W.1ORCID,Castañar Laura17ORCID

Affiliation:

1. Department of Chemistry University of Manchester Manchester M13 9PL UK

2. Current address: GSK Medicines Research Centre Stevenage SG1 2NY UK

3. Current address: Laboratory of Chemical Physics National Institute of Diabetes and Digestive and Kidney Diseases National Institute of Health Maryland 20892 USA

4. Current address: Department of Chemistry University of York York YO10 5DD UK

5. Johnson Matthey Johnson Matthey Technology Centre Sonning Common RG4 9NH UK

6. Current address: JEOL UK Ltd. Long Hanborough OX29 8LJ UK

7. Current address: Department of Organic Chemistry Faculty of Chemical Science Complutense University of Madrid Madrid 28040 Spain

Abstract

AbstractSolution state 1H NMR spectroscopy provides valuable insights into molecular structure and conformation. However, when the spectrum exhibits severe signal overlap, it hampers the extraction of key structural information. Here, an ultraselective, ultrahigh resolution TOCSY method is introduced that greatly reduces spectral complexity, allowing the extraction of previously inaccessible spectral information. It combines the recently developed GEMSTONE excitation with homonuclear decoupling to provide highly simplified through‐bond correlation 1D 1H NMR spectra, showing all signals within the selected spin system as singlets. The new method can greatly facilitate the analysis of mixtures, as shown here for a mixture of Cinchona alkaloids (popular catalysts in asymmetric synthesis) and a mixture of glucocorticoids (used for treating conditions such as asthma).

Funder

Engineering and Physical Sciences Research Council

Comunidad de Madrid

Publisher

Wiley

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