Design of a combined LED and rapid-injection NMR system for structure elucidations and kinetic analyses.

IF 15.7 1区综合性期刊 Q1 MULTIDISCIPLINARY SCIENCES

Nature Communications Pub Date : 2025-10-02 DOI:10.1038/s41467-025-63848-7

Danniel K Arriaga, Ravinder Kaur, Andy A Thomas

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Abstract

Nuclear magnetic resonance (NMR) spectroscopy is a powerful technique often used for structural elucidation of various molecules. The utility of NMR for in situ reaction monitoring is represented by the numerous strategies to conduct chemical reactions inside of the spectrometer, such as rapid-injection (RI-NMR) and LED NMR. In this work, the design of a combined LED and rapid-injection NMR (LED-RI-NMR) apparatus is described and showcased in kinetic studies for three photochemical reactions. The simple design of the LED-RI-NMR system allows for the introduction of both light and reagents into NMR samples for in situ reaction monitoring of reactive intermediates. The distinguishing features of the LED-RI-NMR system described herein include the ability to explore and intercept photogenerated intermediates via RI-NMR and explore the photochemical properties of fleeting intermediates generated by RI-NMR. We demonstrate the versatility of this experimental tool for the kinetic study of organophotoredox cycloadditions, Wolff rearrangements, and azobenzene isomerization reactions.

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用于结构解析和动力学分析的LED和快速注入核磁共振组合系统的设计。

核磁共振波谱是一种强大的技术，经常用于各种分子的结构解析。核磁共振在现场反应监测中的应用体现在许多在光谱仪内进行化学反应的策略，如快速注射（RI-NMR）和LED核磁共振。在这项工作中，结合LED和快速注入核磁共振（LED- ri -NMR）装置的设计被描述并展示在三个光化学反应的动力学研究中。LED-RI-NMR系统的简单设计允许将光和试剂引入NMR样品中，用于活性中间体的原位反应监测。本文描述的LED-RI-NMR系统的显著特征包括通过RI-NMR探索和拦截光生成中间体的能力，以及探索由RI-NMR产生的转瞬即逝中间体的光化学性质的能力。我们证明了该实验工具在有机光氧化还原环加成、沃尔夫重排和偶氮苯异构化反应动力学研究中的多功能性。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Nature Communications Biological Science Disciplines-

CiteScore

24.90

自引率

2.40%

发文量

6928

审稿时长

3.7 months

期刊介绍： Nature Communications, an open-access journal, publishes high-quality research spanning all areas of the natural sciences. Papers featured in the journal showcase significant advances relevant to specialists in each respective field. With a 2-year impact factor of 16.6 (2022) and a median time of 8 days from submission to the first editorial decision, Nature Communications is committed to rapid dissemination of research findings. As a multidisciplinary journal, it welcomes contributions from biological, health, physical, chemical, Earth, social, mathematical, applied, and engineering sciences, aiming to highlight important breakthroughs within each domain.