对映体和手性位移试剂的作用及其纯度测定的1H-NMR研究——BETR法

波谱学杂志 ›› 1990, Vol. 7 ›› Issue (3): 281-288.

对映体和手性位移试剂的作用及其纯度测定的¹H-NMR研究——BETR法

范世彦

中国科学院武汉物理研究所波谱与原子分子物理开放实验室

收稿日期:1989-07-03 修回日期:1989-10-09 出版日期:1990-09-05 发布日期:2018-01-23
基金资助:
国家自然科学基金;武汉波谱与原子分子开放实验室基金

THE STUDY OF THE INTERACTION BETWEEN THE ENANTIOMER AND CHIRAL SHIFT REAGENT IN THE DETERMINATION OF ENANTIOMERIC PURITY——BETR Method

Fan Shiyan

Laboratory of Magn. Reson and Atomic and Mol. Phys. Inst. of Phys. Academia Sinica, Wuhan

Received:1989-07-03 Revised:1989-10-09 Online:1990-09-05 Published:2018-01-23

摘要/Abstract

摘要： BETR法是通过CPMG脉冲系列消除手性位移试剂的宽峰,用¹H-NMR测定对映体含量的一个新而简单的方法。用此法测定了2'-羟基-2-苄氧基-1,1'联萘对映体含量,并发现随着手性位移试剂Eu(hfc)₃/联萘的克分子浓度比的增加,R异构体的亚甲基的二个质子共振峰向低场移动得比S异构体快,但S异构体的亚甲基的二个质子共振峰向低场移动的化学位移差值比R异构体增加快,并提出了由于Bloch-Siegert效应,它们的值都和磁场强度有关。

关键词: BETR定量法, Eu (hfc)₃, 对映体, 手性联萘衍生物, Bloch-Siegert效应

Abstract: A novel and simple ¹H-NMR method for determination of enantiomeric purity, BETR, is studied. BETR (Broad Peak Elimination by T₂ Relaxation) method is one that eliminates the broad peak of chiral shift reagent by CPMG pulse sequence in the ¹H-NMR determination. In the application of this technique to the determination of enantiomeric purity of 2'-hydroxy-2-benzyIoxy-1.1'-binaphthyl (1), in the presence of Eu(hfc)₃, the results are as follows. Increasing the molar ratio of Eu(hfc) l,the resonance peaks of methene in R isomer shift to the lower rede faster than that in S isomers but the chemical shift difference between wo protons of methene in S isomer is greater than that in R isomer. Due to Bloch-Siegert effect, their value:are dependent on the magnetic field strengrh.

Key words: BETR method, Enantiomer, Chiral shift reagent, Chiral binaphthyl derivate, Bloch-Siegert effect

范世彦. 对映体和手性位移试剂的作用及其纯度测定的¹H-NMR研究——BETR法[J]. 波谱学杂志, 1990, 7(3): 281-288.

Fan Shiyan. THE STUDY OF THE INTERACTION BETWEEN THE ENANTIOMER AND CHIRAL SHIFT REAGENT IN THE DETERMINATION OF ENANTIOMERIC PURITY——BETR Method[J]. Chinese Journal of Magnetic Resonance, 1990, 7(3): 281-288.

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对映体和手性位移试剂的作用及其纯度测定的¹H-NMR研究——BETR法

THE STUDY OF THE INTERACTION BETWEEN THE ENANTIOMER AND CHIRAL SHIFT REAGENT IN THE DETERMINATION OF ENANTIOMERIC PURITY——BETR Method

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