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NMR Structural Characterization from One-Bond13 C-13 C Couplings - Complete Assignment of a Hydrogen-poor Depsidone
Magnetic Resonance in Chemistry ( IF 1.9 ) Pub Date : 2020-08-03 , DOI: 10.1002/mrc.5077
Shannon Sestile 1 , David Richardson 1 , Ryan Toomey 2 , Laurence G Cool 3 , James K Harper 4
Affiliation  

The connectivity, conformation, tautomeric form, and dynamics of a new depsidone, perisalazinic acid were characterized using one-bond 13 C-13 C NMR scalar couplings (1 JCC ) obtained from the INADEQUATE experiment. Characterization of perisalazinic acid using more conventional NMR techniques is problematic due to the extremely limited number of C-H protons present. In the present study, 81 candidate structures were considered and a best-fit structure was selected by comparing computed 1 JCC values for each candidate to 15 experimental values. Of the six flexible moieties in perisalazinic acid, three are adequately represented by a single orientation stabilized by intramolecular hydrogen bonding. The three remaining groups are present as mixtures of conformers with two sites consisting of a pair of conformations and another disordered over six orientations. This study demonstrates the feasibility of complete three-dimensional structural characterization of an unknown using only theoretical and experimental 1 JCC values.

中文翻译:

One-Bond13 C-13 C 偶联物的 NMR 结构表征 - 贫氢地塞酮的完整归属

使用从 INADEQUATE 实验中获得的单键 13 C-13 C NMR 标量耦合 (1 JCC) 表征了新的地塞酮、perisalazinic 酸的连接性、构象、互变异构形式和动力学。由于存在的 CH 质子数量极其有限,因此使用更传统的 NMR 技术表征 perisalazinic 酸是有问题的。在本研究中,考虑了 81 个候选结构,并通过将每个候选的计算 1 JCC 值与 15 个实验值进行比较来选择最适合的结构。在 perisalazinic 酸的六个柔性部分中,三个由分子内氢键稳定的单一取向充分代表。剩下的三个基团作为构象异构体的混合物存在,其中两个位点由一对构象组成,另一个在六个方向上无序。这项研究证明了仅使用理论和实验 1 JCC 值对未知物进行完整三维结构表征的可行性。
更新日期:2020-08-03
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