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溶解于[EMIm][OAc]中的SN和(SN)的核磁共振与电子顺磁共振光谱表征

Nuclear Magnetic Resonance- and Electron Paramagnetic Resonance Spectroscopic Characterization of SN and (SN) Dissolved in [EMIm][OAc].

作者信息

Radicke Julian, Jerschabek Vanessa, Hashemi Haeri Haleh, Abu Bakar Muhammad, Hinderberger Dariush, Kressler Jörg, Busse Karsten

机构信息

Department of Chemistry, Martin Luther University Halle-Wittenberg, von-Danckelmann-Platz 4, D-06120 Halle (Saale), Germany.

出版信息

J Phys Chem B. 2025 Apr 24;129(16):4063-4077. doi: 10.1021/acs.jpcb.5c00294. Epub 2025 Apr 10.

Abstract

This work focuses on the reaction mechanism of poly(sulfur nitride) ((SN), (SN)), with the ionic liquid (IL) 1-ethyl-3-methylimidazolium acetate [EMIm][OAc]. We compare this with the reaction of the IL with SN or its N-labeled form SN, a precursor for the synthesis of (SN) and (SN). After purification of the SN-IL- and SN-IL systems via column chromatography, we characterized the reaction products with H, C, and N nuclear magnetic resonance spectroscopy and with electron spray ionization time-of-flight mass spectrometry. Furthermore, time-resolved electron paramagnetic resonance spectroscopy and time-resolved ultraviolet-visible spectroscopy were carried out. Thus, radical intermediates were detected, which were consumed with reaction time. Finally, we postulate a reaction mechanism for the SN-IL- and SN-IL systems and compare this with the respective data for the (SN) -IL- and (SN)-IL-systems.

摘要

这项工作聚焦于聚氮化硫((SN),(SN))与离子液体(IL)1-乙基-3-甲基咪唑醋酸盐[EMIm][OAc]的反应机理。我们将此与该离子液体与SN或其氮标记形式SN((SN)和(SN)合成的前体)的反应进行比较。通过柱色谱法对SN-IL和SN-IL体系进行纯化后,我们利用氢、碳和氮核磁共振光谱以及电喷雾电离飞行时间质谱对反应产物进行了表征。此外,还进行了时间分辨电子顺磁共振光谱和时间分辨紫外可见光谱分析。由此检测到了自由基中间体,其会随着反应时间而消耗。最后,我们推测了SN-IL和SN-IL体系的反应机理,并将其与(SN) -IL和(SN)-IL体系的相应数据进行比较。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/cc52/12035862/8ec77e7d5983/jp5c00294_0009.jpg

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