1α-羟基去氢表雄酮的制备工艺研究
发布时间:2018-04-16 18:34
本文选题:1α-羟基去氢表雄酮 + 1 ; 参考:《佳木斯大学》2014年硕士论文
【摘要】:目的研究1α-羟基去氢表雄酮的制备工艺,获得可工业化生产的制备工艺。 方法以1,4-雄烯二酮为起始原料,经羰基保护、溴代、消除、环氧化、羰基还原、氢化还原、开环及脱保护等8步反应,,制得1α-羟基去氢表雄酮,优化部分合成工艺,经MS、1H-NMR、13C-NMR确证部分中间体及目标产物的结构。 结果完成1α-羟基去氢表雄酮的制备工艺研究,优化了部分工艺;获得目标产物1α-羟基去氢表雄酮,总收率为13.7%。经MS、1H-NMR、13C-NMR确证了部分中间体及目标产物的结构。 结论获得的1α-羟基去氢表雄酮制备工艺具有原料及试剂易得、反应条件易于控制、操作简便等优点,该工艺为工业化规模生产1α-羟基去氢表雄酮奠定了基础。
[Abstract]:Objective to study the preparation process of 1 伪-hydroxyl dehydroepiandrosterone and obtain the industrial production process.Methods 1 伪 -hydroxyl dehydroepiandrosterone was prepared from 1o 4-androstenedione by 8 steps of carbonyl protection, bromination, elimination, epoxidation, carbonyl reduction, hydrogenation reduction, ring-opening and deprotection.The structures of some intermediates and their target products were confirmed by MSN 1H-NMR-13C-NMR.Results the preparation process of 1 伪 -hydroxyl dehydroepiandrosterone was studied and some of the processes were optimized, and the target product 1 伪 -hydroxyl dehydroepiandrosterone was obtained in a total yield of 13.7%.The structures of some intermediates and their target products were confirmed by MSN 1H-NMR-13C-NMR.Conclusion the prepared process of 1 伪 -hydroxyl dehydroepiandrosterone is easy to obtain from raw materials and reagents, easy to control the reaction conditions and easy to operate. This process lays a foundation for the industrial production of 1 伪 -hydroxyl dehydroepiandrosterone.
【学位授予单位】:佳木斯大学
【学位级别】:硕士
【学位授予年份】:2014
【分类号】:R914.5
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