氘标记盐酸埃他卡林的合成及其质谱裂解途径

Synthesis of(N-2H7)iptakalim hydrochloride and its proposed fragment pathways of mass spectroscopy

目的合成盐酸埃他卡林的氘定位标记化合物 ,确证盐酸埃他卡林的质谱裂解途径。方法由 2 ,3 二甲基 2 丁胺与 (N 2 H7)溴代异丙烷缩合而得到氘标记盐酸埃他卡林 ;测定盐酸埃他卡林、(N 2 H7)盐酸埃他卡林及两者混合物的质谱 (EI)。结果利用核磁共振氢谱、质谱、红外光谱和元素分析对目标化合物进行了结构确证。通过对比氘标记和非标记的盐酸埃他卡林的质谱图 ,确定了盐酸埃他卡林的质谱裂解途径。

Aim To synthesize deuterium labelled iptakalim hydrochloride and confirm the MS fragment pathways of iptakalim hydrochloride.Methods The deuterium labelled iptakalim hydrochloride was obtained by the condensation of 2,3-dimethyl-2-butamine with (~2H_7)2-bromopropane.The un-reacted 2,3-dimethyl-2-butamine was derivated to its amide.The (N-~2H_7)iptakalim hydrochloride could be easily separated from the reaction mixture.Results ~1H-NMR,MS,IR and elemental analysis confirmed the structure of(N-~2H_7)iptakalim hydrochloride.The MS fragment pathways of iptakalim hydrochloride were proposed by comparing the mass spectra of iptakalim hydrochloride,(N-~2H_7)iptakalim hydrochloride and the mixture of the two compounds were proposed.Conclusion Mass spectroscopy with isotope labelled compounds as the internal standard provides a convenient method to propose the fragment pathways of drugs.