摘要
目的改进雌激素药物中间体6-酮雌二醇的合成方法。方法以雌酚酮为起始原料经NaBH_4还原、乙酰基保护、Na_2CrO_4氧化、KOH-MeOH溶液水解得到6-酮雌二醇。结果经过4步反应总产率40.9%,目标产物结构经~1HNMR、^(13)C-NMR和MS确证。结论该合成方法原料易得、条件温和、操作简便,适用于试验性的小规模制备。
Objective To improve the synthetic route of 6-oxo-estradiol, an intermediate of estrogen drugs.Methods 6-oxo-estradiol was obtained from estrone by reducing carbonyl with NaBH4, acylating hydroxyl with acetic anhydride,oxidating 6-methylene with Na2CrO4, and by hydrolyzing acetyl with KOH- MeOH.Results The overall yield of target product after the four steps was 40.9%.Moreover, the structure of the target compound was verified by ^1H-NMR,^13 C-NMR and MS. Conclusion This synthetic method requires mild conditions, simple operation and easily available raw materials, which is suitable for smallscale production of preparations in experimental research.
出处
《解放军药学学报》
CAS
CSCD
2017年第1期6-8,共3页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
国家自然科学基金
No.81273431
81072531
21102176
21272273
