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- Title
Application of 1D <sup>15</sup>N and band‐selective 2D <sup>1</sup>H‐<sup>15</sup>N CLIP‐HSQMBC to detect <sup>35/37</sup>Cl isotope effect on nitrogen for unequivocal structure elucidation of the N‐Cl moiety in molecules.
- Authors
Hwang, Tsang‐Lin; Yang, Ning; Cheng, Guilong; Chen, Ying; Cui, Sheng
- Abstract
An impurity, designated MS204, was isolated from a scale‐up production of an intermediate toward the synthesis of an active pharmaceutical ingredient. Structural elucidation of this chloro‐containing impurity was performed based on the analysis of the MS and NMR data. Band‐selective 2D 1H‐15N CLIP‐HSQMBC experiment was developed to unequivocally identify the ionic N‐Cl moiety in the molecule by discovering the two isotope‐shifted nitrogen peaks as 3 to 1 ratio separated by about 1Δ15N(37/35Cl) = 19.6 ppb (1.19 Hz) due to the Cl isotope effect. 1D 15N and 2D 1H‐15N CLIP‐HSQMBC experiments were applied to commercially available compounds to further confirm the techniques by detecting the isotope shift of nitrogen peaks for the N‐Cl moiety in molecules.
- Subjects
NITROGEN isotopes; MOIETIES (Chemistry); ISOTOPE shift; MOLECULES; NITROGEN; ISOTOPES
- Publication
Magnetic Resonance in Chemistry, 2022, Vol 60, Issue 1, p157
- ISSN
0749-1581
- Publication type
Article
- DOI
10.1002/mrc.5204