核磁共振光谱法测定(S)-(-)-α-苯乙胺的对映体纯度  

Determination of Enantiomeric Purity of (S)-(-)-α-phenylethylamine by NMR

作　　者：江向东[1] 苏克曼[2] 蔡水洪[3] 

机构地区：[1]华东理工大学石化学院,201512 [2]上海华东理工大学化学系,200237 [3]上海华东理工大学化工系,上海200237

出　　处：《光谱学与光谱分析》2001年第3期404-405,共2页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金资助!(2 99760 1 6)

摘　　要：以 (2R ,3R) 二苯甲酰酒石酸为手性溶解剂 ,用1HNMR的方法测定了 (S) (- ) α 苯乙胺样品的对映体纯度。以氘代氯仿为溶剂 ,当样品浓度为 0 0 5 1mol·L-1,手性溶解剂与样品的摩尔比为 0 33时 ,α 苯乙胺甲基双峰的化学位移不等价为 0 0 8ppm(基线分离 )。由甲基吸收峰的面积可以计算样品的对映体纯度。测量结果的相对标准偏差与样品的对映体纯度有关 ,当样品的ee值高达 99 1%时 ,RSD为 0 3 % (n =4)。It was reported the determination of enantiomeric purities of (S) (-) α 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 α phenylethylamine was 0 08 ppm(base line separation) in solvent CDCl 3,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 α 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).

关 键 词：核磁共振 对映体纯度 手性溶解剂 (S)-(-)-α-苯乙胺 (2R 3R)-二苯甲酰酒石酸 测定 

分 类 号：O625.631[理学—有机化学] O657.2[理学—化学]