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Direct and indirect hyperpolarisation of amines using parahydrogen†
Chemical Science ( IF 7.6 ) Pub Date : 2018-03-09 00:00:00 , DOI: 10.1039/c8sc00526e
Wissam Iali 1 , Peter J Rayner 1 , Adel Alshehri 1 , A Jonathan Holmes 1 , Amy J Ruddlesden 1 , Simon B Duckett 1
Affiliation  

Nuclear Magnetic Resonance (NMR) and Magnetic Resonance Imaging (MRI) are two widely used techniques for the study of molecules and materials. Hyperpolarisation methods, such as Signal Amplification By Reversible Exchange (SABRE), turn typically weak magnetic resonance responses into strong signals. In this article we detail how it is possible to hyperpolarise the 1H, 13C and 15N nuclei of a range of amines. This involved showing how primary amines form stable but labile complexes of the type [Ir(H)2(IMes)(amine)3]Cl that allow parahydrogen to relay its latent polarisation into the amine. By optimising the temperature and parahydrogen pressure a 1000-fold per proton NH signal gain for deuterated benzylamine is achieved at 9.4 T. Additionally, we show that sterically hindered and electron poor amines that bind poorly to iridium can be hyperpolarised by either employing a co-ligand for complex stabilisation, or harnessing the fact that it is possible to exchange hyperpolarised protons between amines in a mixture, through the recently reported SABRE-RELAY method. These chemical refinements have significant potential to extend the classes of agent that can be hyperpolarised by readily accessible parahydrogen.

中文翻译:

使用仲氢对胺进行直接和间接超极化†

核磁共振 (NMR) 和磁共振成像 (MRI) 是两种广泛使用的分子和材料研究技术。超极化方法,例如可逆交换信号放大 (SABRE),将通常较弱的磁共振响应转变为强信号。在本文中,我们详细介绍了如何使一系列胺的1 H、13 C 和15 N 核超极化。这涉及展示伯胺如何形成稳定但不稳定的 [Ir(H) 2 (IMes)(amine) 3 ]Cl型复合物,使氢将其潜在极化传递到胺中。通过优化温度和氢压力,氘代苄胺在 9.4 T 下实现了每个质子 NH 信号增益 1000 倍。此外,我们表明,与铱结合不良的空间位阻和缺电子胺可以通过使用 co 来超极化。 -用于复杂稳定的配体,或利用最近报道的 SABRE-RELAY 方法可以在混合物中的胺之间交换超极化质子这一事实。这些化学改进具有扩展可通过容易获得的对位氢进行超极化的试剂类别的巨大潜力。
更新日期:2018-03-09
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