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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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