Ultraselective, Ultrahigh Resolution 1D TOCSY

James R.D. Montgomery; Emma L. Gates; Marshall J. Smith; Daniel A. Taylor; Jonathan P. Bradley; Daniel B.G. Berry; Peter Kiraly; Mathias Nilsson; Gareth A. Morris; Ralph W. Adams; Laura Castañar

doi:10.1002/cmtd.202400013

Ultraselective, Ultrahigh Resolution 1D TOCSY

James R.D. Montgomery, Emma L. Gates, Marshall J. Smith, Daniel A. Taylor, Jonathan P. Bradley, Daniel B.G. Berry, Peter Kiraly, Mathias Nilsson, Gareth A. Morris, Ralph W. Adams^*, Laura Castañar^*

^*Corresponding author for this work

Chemistry

Research output: Contribution to journal › Article › peer-review

Abstract

Solution 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).

Original language	English
Article number	e202400013
Number of pages	5
Journal	Chemistry-Methods
Volume	4
Issue number	9
Early online date	7 Aug 2024
DOIs	https://doi.org/10.1002/cmtd.202400013
Publication status	Published - 12 Sept 2024

Bibliographical note

Publisher Copyright:
© 2024 The Author(s). Chemistry - Methods published by Chemistry Europe and Wiley-VCH GmbH.

Keywords

GEMSTONE
Mixture Analysis
NMR Spectroscopy
Pure Shift
TOCSY

Access to Document

10.1002/cmtd.202400013Licence: CC BY

Chemistry Methods - 2024 - Montgomery - Ultraselective Ultrahigh Resolution 1D TOCSY
© 2024 The Author(s).
Final published version, 0.98 MBLicence: CC BY

Cite this

@article{691af31c3f174b7a9284d6b29c91d1e4,

title = "Ultraselective, Ultrahigh Resolution 1D TOCSY",

abstract = "Solution 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).",

keywords = "GEMSTONE, Mixture Analysis, NMR Spectroscopy, Pure Shift, TOCSY",

author = "Montgomery, {James R.D.} and Gates, {Emma L.} and Smith, {Marshall J.} and Taylor, {Daniel A.} and Bradley, {Jonathan P.} and Berry, {Daniel B.G.} and Peter Kiraly and Mathias Nilsson and Morris, {Gareth A.} and Adams, {Ralph W.} and Laura Casta{\~n}ar",

note = "Publisher Copyright: {\textcopyright} 2024 The Author(s). Chemistry - Methods published by Chemistry Europe and Wiley-VCH GmbH.",

year = "2024",

month = sep,

day = "12",

doi = "10.1002/cmtd.202400013",

language = "English",

volume = "4",

journal = "Chemistry-Methods",

issn = "2628-9725",

publisher = "John Wiley and Sons Inc.",

number = "9",

}

TY - JOUR

T1 - Ultraselective, Ultrahigh Resolution 1D TOCSY

AU - Montgomery, James R.D.

AU - Gates, Emma L.

AU - Smith, Marshall J.

AU - Taylor, Daniel A.

AU - Bradley, Jonathan P.

AU - Berry, Daniel B.G.

AU - Kiraly, Peter

AU - Nilsson, Mathias

AU - Morris, Gareth A.

AU - Adams, Ralph W.

AU - Castañar, Laura

PY - 2024/9/12

Y1 - 2024/9/12

N2 - Solution 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).

AB - Solution 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).

KW - GEMSTONE

KW - Mixture Analysis

KW - NMR Spectroscopy

KW - Pure Shift

KW - TOCSY

UR - http://www.scopus.com/inward/record.url?scp=85200563462&partnerID=8YFLogxK

U2 - 10.1002/cmtd.202400013

DO - 10.1002/cmtd.202400013

M3 - Article

AN - SCOPUS:85200563462

SN - 2628-9725

VL - 4

JO - Chemistry-Methods

JF - Chemistry-Methods

IS - 9

M1 - e202400013

ER -

Ultraselective, Ultrahigh Resolution 1D TOCSY

Abstract

Bibliographical note

Keywords

Access to Document

Other files and links

Cite this