维库溴胺合成中的6个中间体均为雄甾类化合物,我们以重要中间体2β,16β-二(1-哌啶基)-5α-雄甾烷-3α,17β-二醇为例,使用质谱、红外光谱和核磁共振技术确定了它的结构,并结合^1H NMR,^13C NMR,DEPT,^1H-^1H COSY,HSQC,HMBC多种核磁共振分析方法,详细归属了其所有的^1H NMR和^13C NMR数据,利用ROESY确定了其相对构型.根据相同方法,归属了其它5个中间体的^13C NMR数据,为它们的结构鉴定提供了重要依据,为维库溴铵合成工艺的中间体质量控制提供了参考数据.
2β, 16β-dipieridino-5α-androstan-3α, 17β-diol is an important intermediate in the synthesis of vecuronium bromide. In this study, the molecular structure of the compound was elucidated by MS, IR, 1D NMR and 2D NMR techniques (i. e. , ^1H NMR, ^13C NMR, DEPT, ^1H-^1H COSY, HSQC and HMBC). The stereochemistry conformation of the compound was confirmed by ROESY experiments. The ^13C NMR chemical shifts of five other androstan intermediates were also assigned.