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[通过核磁共振法测定(S)-(-)-α-苯乙胺的对映体纯度]

[Determination of enantiomeric purity of (S)-(-)-alpha-phenylethylamine by NMR].

作者信息

Jiang X, Su K, Cai S

机构信息

Petrochemical Institute, ECUST, 201512 Shanghai.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2001 Jun;21(3):404-5.

Abstract

It was reported the determination of enantiomeric purities of (S)-(-)-alpha-phenylethylamine by 1H NMR, using (2R, 3R)-dibenzoyl-tartaric acid as chiral solvating agent. 1H NMR chemical shift non-equivalence of the methyl doublet of alpha-phenylethylamine was 0.08 ppm(base-line separation) in solvent CDCl3, when the concentration of the sample was 0.051 mol.L-1, the molar ratio between chiral solvating agent and the sample was 0.33. The enantiomeric purities could be determined by the peak areas of the methyl doublet of alpha-phenylethylamine. The relative standard deviation depended upon the enantiomeric purities of sample. With enantiomeric purities as high as 99.1% ee, the RSD was 0.3% (n = 4).

摘要

据报道,使用(2R, 3R)-二苯甲酰酒石酸作为手性溶剂化剂,通过1H NMR测定(S)-(-)-α-苯乙胺的对映体纯度。在溶剂CDCl3中,当样品浓度为0.051 mol·L-1,手性溶剂化剂与样品的摩尔比为0.33时,α-苯乙胺甲基双峰的1H NMR化学位移非等价性为0.08 ppm(基线分离)。对映体纯度可通过α-苯乙胺甲基双峰的峰面积来确定。相对标准偏差取决于样品的对映体纯度。对映体纯度高达99.1% ee时,相对标准偏差为0.3%(n = 4)。

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