摘要
目的合成甲基泼尼松龙的一个手性杂质6β-甲基泼尼松龙,作为有关物质质量控制的对照品。方法以5α,6α-环氧-11β,17α-二羟基孕甾-3,20-二乙二醇缩酮为原料,经环氧开环、酸性水解、碱性消除、生物脱氢、碘代、置换、碱性水解以及制备液相纯化得到高纯度的6β-甲基泼尼松龙。结果目标产物结构经1H-NMR、13C-NMR、NOESY和MS确证,纯度经HPLC检测达到99.8%。结论该杂质可作为甲基泼尼松龙原料药质量控制的杂质对照品。
OBJECTIVE To synthesize 6β-methylprednisolone, a chiral impurity of methylprednisolone, as a reference substance for the quality control. METHODS High purity 6β-methylprednisolone was synthesized from 5α, 6α-epoxy^-11β, 17α-dihydroxypregna-3, 20-dione-3, 20-bis（ethyleneketal） through epoxide ring-opening, acidic hydrolysis, alkaline elimination, fermented dehydrogenation, iodination, substitution, alkaline hydrolysis and purification by the preparative HPLC technique. RESULTS The structure of desired product was confirmed by 1 H-NMR, 13 C-NMR, NOESY and MS. The purity was 99.8% as determined by HPLC. CONCLUSION The synthetic impurity can be used as the reference substance of the impurity in the quality control of the methylprednisolone.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2018年第8期1150-1153,共4页
Chinese Journal of Modern Applied Pharmacy
