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罗库溴铵(Rocuronium Bromide)是新的手术前的甾醇类肌松药,其安全性和有效性已得到临床研究和应用的证实.雄甾-3,17-二醇(1)是合成罗库溴铵的关键中间体.用硼氢化钠还原(2α,3α,5α,16β)-2,3-环氧基-16-(1-吡咯)-17-氧代雄甾烷(2),然后在吗啉和水中回流使环氧开环得到雄甾-3,17-二醇(1).高分辨TOF-MS质谱和1H NMR,13C NMR,1H-1H COSY,HSQC,DEPT,HMBC,2D NOESY等核磁共振谱表征确认其分子构造,并且制备和测定了雄甾-3,17-二醇1的单晶结构,确认了它的立体构型.雄甾-3,17-二醇(1)的样品的X粉末衍射分析研究表明其衍射谱与根据单晶数据计算的理论谱一致,因此,合成的雄甾-3,17-二醇(1)的分子结构是(2β,3α,5α,16β,17β)-2-(4-吗啉基)-16-(1-吡咯)雄甾-3,17-二醇,其立体构型与罗库溴铵的立体构型一致.
Rocuronium Bromide is a new preoperative steroid muscle relaxant, its safety and effectiveness have been confirmed by clinical research and application of androst-3,17-diol (1) is a synthetic Luo (2α, 3α, 5α, 16β) -2,3-epoxy-16- (1-pyrrole) -17-oxoandrostane (2) was reduced with sodium borohydride, Followed by ring-opening of the epoxy in morpholine and water to give the androst-3,17-diol (1) .High resolution TOF-MS and 1H NMR, 13C NMR, 1H-1H COZY, HSQC, DEPT, HMBC, 2D NOESY and other nuclear magnetic resonance spectroscopy confirmed its molecular structure, and the preparation and determination of androst-3,17-diol 1 single crystal structure confirmed its stereostructure. Androst-3,17-diol ( 1) showed that the diffraction spectrum was in agreement with the theoretical spectrum calculated from the single crystal data. Therefore, the molecular structure of the synthesized androsta-3,17-diol (1) was (2β, 3α, 5α, 16β, 17β) -2- (4-morpholinyl) -16- (1-pyrrole) androst-3,17-diol, whose stereoconfiguration is consistent with the stereoconfiguration of rocuronium.