一种可靠的外部校准方法,用于用基板NMR监测反应
Tristan Maschmeyer1,2, Breanna Conklin1, Thomas C Malig1
1Synthetic Molecule Pharmaceutical Sciences, Genentech Inc., South San Francisco, California, USA.
Magnetic resonance in chemistry : MRC
|December 20, 2023
概括
使用外部校准的定量NMR (qNMR) 提供了一种可靠的反应监测方法. 这种技术应用于胺合反应和基板NMR,为流程优化提供实时数据.
科学领域:
- 分析化学 分析化学
- 频谱学是一种光谱学.
背景情况:
- 核磁共振 (NMR) 光谱对于分析化学样品至关重要.
- 具有内部标准的定量NMR (qNMR) 是常见的,但外部校准避免了样本干扰.
- 基板NMR光谱仪虽然容易使用,但存在诸如共振重叠等挑战.
研究的目的:
- 为定量NMR (qNMR) 开发一个强大的外部校准方法.
- 应用这种qNMR技术来使用基板NMR系统监测具有药学意义的胺合反应.
主要方法:
- 开发了一种使用单分析和多分析线性回归来确定NMR系统度转换因子的方法.
- 采用在线停止流动的基板NMR系统来监测反应动力学.
- 研究的1.1'-carbonyldiimidazole (CDI) 促进了酸激活和随后的胺合.
主要成果:
- 成功建立了一种简单而强大的方法,用于在qNMR中进行外部校准.
- 证明了基板NMR用于实时反应监测的能力.
- 在胺合过程中量化关键步骤,提供可操作的数据.
结论:
- 用qNMR进行外部校准是内部标准的一个有价值的替代方案,尤其对于复杂的样品和基板仪器.
- 在线停止流量基板NMR能够实时对化学反应进行定量分析.
- 这种方法使分析师能够在化学过程中做出明智的决策.
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