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机构地区:[1]大连理工大学精细化工国家重点实验室,大连116012
出 处:《分析化学》2003年第6期659-663,共5页Chinese Journal of Analytical Chemistry
摘 要:从工业和合成产品脂肪胺聚氧乙基醚中用TLC和快速色谱 (FC)分离精制得到 6个脂肪胺聚氧乙基醚模型化合物 ,用1 H、1 3C、gCOSY ,gHSQC和gHMBC等核磁共振波谱和质谱表征了其结构 ,完成了1 H和1 3CNMR谱带的归属 ,为本系列化合物的结构和EO分布鉴定提供了依据 ,并给出了计算本系列化合物叔胺值的方法。考察了酸性条件对脂肪胺聚氧乙基醚化合物相关基团化学位移的影响。Six model compounds of polyoxyethylene alkyl amines were refuted and purified through the method of thin layer chromatography (TLC) and flash chromatography (FC) from different industrial products. Their structures and composition have been studied by H-1, C-13, gradient correlated spectroscopy, gradient H-1-detested heternuclear single quantum coherence and gradient H-1-detected heter-nuclear multiple bond coherence spectra combined with mass spectrometry (MS). The assignments of H-1 and C-13 nuclear magnetic resonance (NMR) absorptions have provided the foundation to characterize the structures and polyoxyethylene ether (EO) distribution. in the molecules. Method to calculate the percentage of tertiary amine was worked out based on quantitative data in NMR spectra. Acidic influence on polyoxyethylene alkyl amines was inspected, which should be noted and can be employed in analyzing this kind of chemicals.
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