| 引用本文: | 应明华,刘东华,胡卫红.6β-甲基泼尼松龙的合成[J].中国现代应用药学,2018,35(8):1150-1153. |
| YING Minghua,LIU Donghua,HU Weihong.Synthesis of 6β-Methylprednisolone[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(8):1150-1153. |
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| 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。 |
| 关键词: 甲基泼尼松龙 6β-甲基泼尼松龙 药物杂质 6β-甲基 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.08.007 |
| 分类号:R914.2 |
| 基金项目: |
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| Synthesis of 6β-Methylprednisolone |
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Ying minghua,liu donghua and Hu weihong
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Zhejiang Xianju Pharmaceutical Co., Ltd.,Zhejiang Xianju Pharmaceutical Co., Ltd.,Zhejiang Xianju Pharmaceutical Co., Ltd.
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| Abstract: |
| 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 1H-NMR, 13C-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. |
| Key words: methylprednisolone 6β-methylprednisolone drug impurity 6β-methyl |
