用于手性二醇对映体纯度核磁共振分析的简单方案。
Simple protocols for NMR analysis of the enantiomeric purity of chiral diols.
作者信息
Kelly Andrew M, Pérez-Fuertes Yolanda, Fossey John S, Yeste Sonia Lozano, Bull Steven D, James Tony D
机构信息
Department of Chemistry, University of Bath, Bath BA2 7AY, UK.
出版信息
Nat Protoc. 2008;3(2):215-9. doi: 10.1038/nprot.2007.523.
A three-component chiral derivatization protocol for determining the enantiopurity of chiral diols by (1)H NMR spectroscopic analysis is described here. The present approach involves the derivatization of 1,2- 1,3- and 1,4-diols with 2-formylphenylboronic acid and enantiopure alpha-methylbenzylamine. This method affords a mixture of diastereoisomeric iminoboronate esters whose ratio can be determined by integration of well-resolved diastereotopic resonances in their (1)H NMR spectra, thus enabling the determination of the enantiopurity of the parent diol. The protocol as described takes less than 90 min to complete.
本文描述了一种用于通过¹H NMR光谱分析测定手性二醇对映体纯度的三组分手性衍生化方案。目前的方法涉及用2-甲酰基苯硼酸和对映体纯的α-甲基苄胺对1,2-、1,3-和1,4-二醇进行衍生化。该方法得到非对映异构亚氨基硼酸酯的混合物，其比例可通过在¹H NMR光谱中对分辨率良好的非对映异位共振进行积分来确定，从而能够测定母体二醇的对映体纯度。所述方案完成时间不到90分钟。
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