The resolution of asymmetrically substituted dibenzophospholes via chromatographic separation of their cyclopalladium derivatives is described for the first time. The absolute configuration of the phosphorus atom was determined by X-ray crystallographic analysis in one case. A general NMR criterion for the complete determination of the configuration of this group of products is proposed. The enantiomeric excess of the resolved compounds was determined by NMR Eu(III) chemical displacement experiments and by HPLC using a chiral stationary phase. (C) 2001 Elsevier Science Ltd. All rights reserved.
机构:
Novartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USANovartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USA
Gao, Jinhai
Rajan, Srinivasan
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Novartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USANovartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USA
Rajan, Srinivasan
Wang, Bing
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Novartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USANovartis Inst Biomed Res Inc, Global Discovery Chem, Cambridge, MA 02139 USA