Application of 1D 15N and band-selective 2D 1H-15N CLIP-HSQMBC to detect 35/37Cl isotope effect on nitrogen for unequivocal structure elucidation of the N-Cl moiety in molecules,Magnetic Resonance in Chemistry

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Application of 1D 15N and band-selective 2D 1H-15N CLIP-HSQMBC to detect 35/37Cl isotope effect on nitrogen for unequivocal structure elucidation of the N-Cl moiety in molecules
Magnetic Resonance in Chemistry ( IF 1.9 ) Pub Date : 2021-08-10 , DOI: 10.1002/mrc.5204
Tsang-Lin Hwang ₁ , Ning Yang ₁ , Guilong Cheng _{1,

2} , Ying Chen _{3,

4} , Sheng Cui _{3,

5}

Affiliation

An impurity, designated MS204, was isolated from a scale-up production of an intermediate toward the synthesis of an active pharmaceutical ingredient. Structural elucidation of this chloro-containing impurity was performed based on the analysis of the MS and NMR data. Band-selective 2D ¹H-¹⁵N CLIP-HSQMBC experiment was developed to unequivocally identify the ionic N-Cl moiety in the molecule by discovering the two isotope-shifted nitrogen peaks as 3 to 1 ratio separated by about ¹Δ¹⁵N(^37/35Cl) = 19.6 ppb (1.19 Hz) due to the Cl isotope effect. 1D ¹⁵N and 2D ¹H-¹⁵N CLIP-HSQMBC experiments were applied to commercially available compounds to further confirm the techniques by detecting the isotope shift of nitrogen peaks for the N-Cl moiety in molecules.

中文翻译：

应用 1D 15N 和带选择性 2D 1H-15N CLIP-HSQMBC 检测 35/37Cl 同位素对氮的影响，以明确分子中 N-Cl 部分的结构阐明

从中间体的放大生产中分离出一种杂质，称为 MS204，以合成活性药物成分。这种含氯杂质的结构解析是基于 MS 和 NMR 数据的分析进行的。开发了带选择性 2D ¹ H- ¹⁵ N CLIP-HSQMBC 实验，通过发现两个同位素位移的氮峰以 3 比 1 的比例相隔约¹ Δ ¹⁵ N( ^{37 /35} Cl) = 19.6 ppb (1.19 Hz) 由于 Cl 同位素效应。1D ¹⁵ N 和 2D ¹ H- ¹⁵N CLIP-HSQMBC 实验应用于市售化合物，通过检测分子中 N-Cl 部分的氮峰的同位素位移来进一步证实该技术。

更新日期：2021-08-10

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