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Determination of enantiomeric purity from solid-state 31P MAS NMR of organophosphorus compounds

✍ Scribed by Knut Vendelboe Andersen; Henrik Bildsøe; Hans Jorgen Jakobsen

Publisher: John Wiley and Sons
Year: 1990
Tongue: English
Weight: 426 KB
Volume: 28
Category: Article
ISSN: 0749-1581
DOI: 10.1002/mrc.1260281310

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✦ Synopsis

Abstract

Phosphorus‐31 Magic‐Angle Spinning (MAS) NMR is shown to be an extremely useful and accurate method for the determination of the enantiomeric purity for chiral organophosphorus compounds. ^31^P and ^13^C chemical shielding tensors in racemic and enantiomeric crystals of organophosphorus compounds vary because of different crystal symmetries. This implies that solid‐state ^31^P (^13^C) MAS spectra of an enantiomerically impure sample reveal separate signals from the racemic and enantiomer crystallites. Simple integration (or deconvolution) of the MAS NMR signals can thus be used to determine the enantiomeric purity of the sample. For organophosphorus compounds the application of this technique to ^31^P MAS NMR is of particular interest due to the high sensitivity and large shielding anisotropy of the ^31^P nucleus.

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