Harnessing polarisation transfer to indazole and imidazole through signal amplification by reversible exchange to improve their NMR detectability.
Harnessing polarisation transfer to indazole and imidazole through signal amplification by reversible exchange to improve their NMR detectability.
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DOI：
10.1002/mrc.4607
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发表时间：
2017-10
期刊：
影响因子：
--
通讯作者：
Duckett SB
中科院分区：
文献类型：
--
作者：
Fekete M;Rayner PJ;Green GGR;Duckett SB
利用可逆交换（SABRE）的信号放大方法，通过预催化剂[IrCl(COD)(IMes)]和[IrCl(COD)(SIMes)]的作用，在共配体乙腈的存在下，对底物吲哚唑和咪唑进行了超极化。还研究了这些催化剂的2H标记形式。我们对两种预催化剂[IrCl(COD)(IMes)]和[IrCl(COD)(SIMes)]的比较，加上N -杂环碳烯的2H标记以及相关的弛豫和极化场变化研究，证明了这些参数在控制可逆交换信号放大效率方面发挥的关键和共同作用。最终，对于咪唑，在400 MHz时每个质子产生700倍的1h信号增益，而对于茚唑，每个质子增加90倍。在这些测量中，共配体乙腈被证明最佳地表现出每质子190倍的信号增益，相关研究揭示了底物在控制该值方面的重要性。版权所有©2017作者。《化学磁共振》由John Wiley & Sons有限公司出版。
The signal amplification by reversible exchange (SABRE) approach has been used to hyperpolarise the substrates indazole and imidazole in the presence of the co‐ligand acetonitrile through the action of the precataysts [IrCl(COD)(IMes)] and [IrCl(COD)(SIMes)]. 2H‐labelled forms of these catalysts were also examined. Our comparison of the two precatalysts [IrCl(COD)(IMes)] and [IrCl(COD)(SIMes)], coupled with 2H labelling of the N‐heterocyclic carbene and associated relaxation and polarisation field variation studies, demonstrates the critical and collective role these parameters play in controlling the efficiency of signal amplification by reversible exchange. Ultimately, with imidazole, a 700‐fold1H signal gain per proton is produced at 400 MHz, whilst for indazole, a 90‐fold increase per proton is achieved. The co‐ligand acetonitrile proved to optimally exhibit a 190‐fold signal gain per proton in these measurements, with the associated studies revealing the importance the substrate plays in controlling this value. Copyright © 2017 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.
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影响因子：
4.6
作者：
Fekete M;Bayfield OW;Duckett SB;Hart S;Mewis RE;Pridmore N;Rayner PJ;Whitwood A
通讯作者：
Whitwood A
影响因子：
4
作者：
Fekete, M.;Gibard, C.;Duckett, S. B.
通讯作者：
Duckett, S. B.
影响因子：
3.3
作者：
Mewis, Ryan E.;Green, Richard A.;Williamson, David C.
通讯作者：
Williamson, David C.
影响因子：
15
作者：
Lloyd, Lyrelle S.;Adams, Ralph W.;Sleigh, Christopher J.
通讯作者：
Sleigh, Christopher J.
影响因子：
16.6
作者：
Eshuis, Nan;Aspers, Ruud L. E. G.;Tessari, Marco
通讯作者：
Tessari, Marco