Centre for NMR & Structural Chemistry, CSIR-Indian Institute of Chemical Technology, Uppal Road, Tarnaka, Hyderabad, 500007, India.
UM-DAE Centre for Excellence in Basic Sciences, University of Mumbai, Kalina Campus, Santa Cruz, Mumbai, 400098, India.
Magn Reson Chem. 2018 Oct;56(10):941-946. doi: 10.1002/mrc.4726. Epub 2018 Mar 25.
J scalar couplings carry rich structural information and their measurements are fundamental in the H NMR based elucidation of small and medium molecules, which, however, are hampered in the presence of large J-coupling network. Further, enhanced spectral resolution is often essential for precise determination of a specific set of H- H J-couplings among the complex J-multiplets. In the light of the recent advancements in homodecoupling pure shift strategies, here, we report absorption mode, band-selective refocused pure shift spin-echo method, which helps in determining H- H J-couplings from crowded spectral regions. The importance of the present band-selective refocused pure shift spin-echo experiment is exemplified for 2 steroid molecules, estradiol and testosterone.
J 核自旋偶合常数携带丰富的结构信息,其测量对于基于 1H NMR 的小分子和中等分子结构阐明至关重要,但在存在大的 J 偶合网络的情况下会受到阻碍。此外,在复杂的 J 多重峰中精确确定特定的一组 1H-1H J 偶合常数,通常需要增强谱分辨率。鉴于同核去耦纯位移策略的最新进展,在此,我们报告了吸收模式、带选择性重聚焦纯位移自旋回波方法,该方法有助于确定拥挤谱区的 1H-1H J 偶合常数。本带选择性重聚焦纯位移自旋回波实验的重要性通过 2 种甾体分子,雌二醇和睾酮举例说明。