二（乙二醇）甲基醚甲基丙烯酸酯（DEGMEMA）衍生的凝胶使甲醇中的小分子排列整齐。

Di(ethylene glycol) methyl ether methacrylate (DEGMEMA)-derived gels align small organic molecules in methanol.

作者信息

García Manuela E, Woodruff Shannon R, Hellemann Erich, Tsarevsky Nicolay V, Gil Roberto R

机构信息

Department of Chemistry, Carnegie Mellon University, 4400 Fifth Avenue, Pittsburgh, PA, 15213, USA.

Department of Organic Chemistry, National University of Cordoba, Medina Allende y Haya de La Torre, Cordoba, 5000, Argentina.

出版信息

Magn Reson Chem. 2017 Mar;55(3):206-209. doi: 10.1002/mrc.4400. Epub 2016 Jan 13.

DOI:10.1002/mrc.4400

PMID:26763068

Abstract

Residual dipolar couplings (RDCs) constitute an important NMR parameter for structural elucidation in all areas of chemistry. In this study, di(ethylene glycol) methyl ether methacrylate (DEGMEMA)-based gels are introduced as alignment media for the measurement of RDCs of small organic molecules in polar solvents such as methanol. The low viscosity of methanol permits the execution of J-scaled BIRD HSQC experiments that yield very sharp lines in anisotropic conditions. The gels have excellent mechanical properties, and their compression and expansion in the swollen state can be reversed and performed multiple times. This process enables the easy loading and release of analytes. The excellent performance of these new aligning gels is demonstrated by analyzing the structure of the alkaloid retrorsine. Copyright © 2016 John Wiley & Sons, Ltd.

摘要

残余偶极耦合（RDCs）是化学各领域中用于结构解析的重要核磁共振参数。在本研究中，引入了基于二（乙二醇）甲基醚甲基丙烯酸酯（DEGMEMA）的凝胶作为取向介质，用于测量极性溶剂（如甲醇）中有机小分子的RDCs。甲醇的低粘度使得能够进行J尺度的BIRD-HSQC实验，该实验在各向异性条件下能产生非常尖锐的谱线。这些凝胶具有优异的机械性能，其在溶胀状态下的压缩和膨胀可以逆转且能多次进行。这一过程便于分析物的轻松加载和释放。通过分析生物碱倒千里光碱的结构，证明了这些新型取向凝胶的优异性能。版权所有© 2016约翰威立父子有限公司。