Department of Chemistry, University of Minnesota, 207 Pleasant Street, SE, Minneapolis, Minnesota 55455, United States.
J Org Chem. 2022 May 6;87(9):5660-5667. doi: 10.1021/acs.joc.1c03127. Epub 2022 Apr 20.
Here we provide examples that demonstrate the value of using properly designed and easily performed doping experiments to give insights about the nature of the analyte(s) present in a H NMR sample. Two mixtures, the first quite complex and the second far less so, have been chosen: (i) the crude pyrolysate from reaction of butyric acid in (supercritical) water at 600 °C and (ii) a mixture of two basic amines. In the former, 13 distinct carbonyl-containing compounds, ranging in relative concentration of nearly 2 orders of magnitude, were positively identified. The latter highlights the advantage of using a doping experiment as opposed to merely comparing the spectra from two separate samples containing the same analyte.
在这里，我们提供了一些示例，展示了使用设计合理且易于执行的掺杂实验来深入了解 H NMR 样品中存在的分析物本质的价值。我们选择了两种混合物，第一种较为复杂，第二种则简单得多：（i）在 600°C 的（超临界）水中丁酸反应的粗热解产物，以及（ii）两种碱性胺的混合物。在前者中，我们鉴定出了 13 种不同的含羰基化合物，其相对浓度相差近 2 个数量级。后者则突出了使用掺杂实验的优势，相比于仅仅比较两个含有相同分析物的单独样品的光谱。
