Real time band selective F1‐decoupled proton NMR for the demixing of overlay spectra of chiral molecules |
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Authors: | Nilamoni Nath Ajay Verma Bikash Baishya Chunni Lal Khetrapal |
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Institution: | 1. Department of NMR‐based Structural Biology, Max Planck Institute for Biophysical Chemistry, Goettingen, GermanyTo whom the correspondence should be addressed.;2. Centre of Biomedical Research, SGPGIMS Campus, Lucknow, U. P., India |
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Abstract: | The small chemical shift dispersion and complex multiplicity pattern in proton NMR limit quantifications, for instance the determination of enantiomeric excess (ee) for an enantiomeric mixture. Herein, we present a simple proton–proton correlation experiment with band selective homonuclear (BASH) decoupling in both F1 and F2 dimensions, for the removal of scalar and residual dipolar couplings to provide collapsed singlet for each chemical site. The method has been demonstrated to separate the severely overlapped spectra of enantiomers using both chiral isotropic and anisotropic phases as well as a small biomolecule, particularly for the diastereotopic protons and also for the determination of ee. Copyright © 2016 John Wiley & Sons, Ltd. |
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Keywords: | Chiral discrimination Pure shift NMR Chiral liquid crystal Lanthanide shift reagent |
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