Beguin Laetitia, Courtieu Jacques, Ziani Latifa, Merlet Denis
Laboratoire de RMN en milieu orienté, Univ. Paris-Sud XI, ICMMO, UMR 8182 CNRS, 91405, Orsay Cedex, France.
Magn Reson Chem. 2006 Dec;44(12):1096-101. doi: 10.1002/mrc.1905.
This work presents a technique to simplify overcrowded proton spectra in chiral liquid crystal solvents using rotation of the sample near the magic angle, VASS, combined with homonuclear selective refocusing 2D NMR experiments, SERF. This methodology provides a powerful tool to visualise enantiomers out of unresolved proton spectra. A modified SERF sequence is presented where the resulting 2D spectrum can be phased to increase the resolution. Accurate enantiomeric excesses are determined that are not possible to measure on static samples. Two examples are presented.
这项工作提出了一种技术,即在近魔角旋转样品的情况下,使用可变角度自旋边带(VASS),结合同核选择性重聚焦二维核磁共振实验(SERF),来简化手性液晶溶剂中过度拥挤的质子谱。该方法提供了一个强大的工具,用于从未解析的质子谱中可视化对映体。本文提出了一种改进的SERF序列,其所得二维谱可以进行相位调整以提高分辨率。确定了准确的对映体过量,这在静态样品上是无法测量的。文中给出了两个例子。