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通过凝胶相高分辨魔角旋转1H核磁共振光谱监测基于二酰亚胺的树脂连接轮烷的热力学控制形成过程。

Monitoring the thermodynamically-controlled formation of diimide-based resin-attached rotaxanes by gel-phase HR MAS 1H NMR spectroscopy.

作者信息

Mullen Kathleen M, Johnstone Ken D, Webb Matthew, Bampos Nick, Sanders Jeremy K M, Gunter Maxwell J

机构信息

Department of Chemistry, School of Science and Technology, the University of New England, Armidale, NSW 2351, Australia.

出版信息

Org Biomol Chem. 2008 Jan 21;6(2):278-86. doi: 10.1039/b716325h. Epub 2007 Dec 6.

DOI:10.1039/b716325h
PMID:18174997
Abstract

The thermodynamically controlled self-assembly of rotaxane and pseudorotaxane systems consisting of (i) a naphthodiimide thread unit terminated at one end with a pyridine ligand, and covalently linked at the other to a gel-phase polystyrene resin support, (ii) a dinaphtho-crown ether shuttle unit, and (iii) a ruthenium carbonyl metalloporphyrin stopper unit, is investigated by high resolution magic angle spinning proton (HR MAS 1H) NMR spectroscopy. The effects of variable concentration of the solution-phase components, the temperature, and added Li+ and Na+ ions are described, and the limitations of the technique are addressed. The dynamic behaviour is compared directly to the solution-phase analogues, where a bulky stopper group is substituted for the polystyrene resin bead.

摘要

通过高分辨率魔角旋转质子(HR MAS 1H)核磁共振光谱研究了由以下部分组成的轮烷和准轮烷体系的热力学控制自组装:(i)一端以吡啶配体封端、另一端与凝胶相聚苯乙烯树脂载体共价连接的萘二酰亚胺线单元,(ii)二萘并冠醚穿梭单元,以及(iii)羰基钌金属卟啉封端单元。描述了溶液相组分浓度变化、温度以及添加Li+和Na+离子的影响,并讨论了该技术的局限性。将动态行为与溶液相类似物直接进行比较,在溶液相类似物中,用一个庞大的封端基团取代了聚苯乙烯树脂珠。

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