Mycroft Coral, Smith Marshall J, Nilsson Mathias, Morris Gareth A, Castañar Laura
Department of Chemistry, University of Manchester, Manchester, UK.
Department of Organic Chemistry, Faculty of Chemical Science, Complutense University of Madrid, Madrid, Spain.
Magn Reson Chem. 2023 Nov;61(11):606-614. doi: 10.1002/mrc.5393. Epub 2023 Sep 9.
NMR measurements of molecules containing sparse fluorine atoms are becoming increasingly common due to their prevalence in medicinal chemistry. However, the presence of both homonuclear and heteronuclear scalar couplings severely complicates their analysis by NMR. In complex systems, FESTA, a heteronuclear spectral editing method, allows simplified H NMR spectra to be obtained containing only H signals from the same spin system as a chosen F. Despite spectral simplification, signal overlap due to the presence of scalar couplings is often a problem in FESTA spectra. Here, we report a new experiment that combines FESTA and pure shift methods to provide fully decoupled ultra-high resolution FESTA spectra showing a single signal for each H chemical environment. The utility of the method is demonstrated for the analysis of two complex fluorine-containing mixtures of pharmaceutical and biochemical interest.
由于含稀疏氟原子的分子在药物化学中普遍存在，对其进行核磁共振（NMR）测量变得越来越常见。然而，同核和异核标量耦合的存在严重复杂化了通过NMR对它们的分析。在复杂体系中，异核光谱编辑方法FESTA能得到简化的¹H NMR谱，其中仅包含与所选¹⁹F来自同一自旋体系的¹H信号。尽管光谱得到了简化，但由于标量耦合的存在，信号重叠在FESTA谱中常常是个问题。在此，我们报道了一项新实验，该实验将FESTA与纯位移方法相结合，以提供完全去耦的超高分辨率FESTA谱，每个¹H化学环境显示为单个信号。该方法的实用性在分析两种具有药物和生化意义的复杂含氟混合物中得到了证明。
