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Determination of enantiomeric purity from solid‐state 31 P MAS NMR of organophosphorus compounds
Author(s) -
Andersen Knut Vendelboe,
Bildsøe Henrik,
Jakobsen Hans Jorgen
Publication year - 1990
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1260281310
Subject(s) - chemistry , enantiomer , magic angle spinning , solid state nuclear magnetic resonance , phosphorus 31 nmr spectroscopy , nmr spectra database , nuclear magnetic resonance spectroscopy , stereochemistry , spectral line , nuclear magnetic resonance , physics , astronomy
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.