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本文主要介绍了17α-乙炔雌三醇合成中增加一步酯化反应,可提高重排物3,16α-二乙酰氧基-雌甾-1,3,5(10)-三烯-17-酮的收率,并保证了乙炔化前体的质量。重排物与乙炔溴化镁反应,生成17α-及17β-两种立体异构体,分离时,将缩丙酮反应改为在半固态下进行,并用乙酸乙酯精制,可不需柱层析分离,既简化了操作,又节省了溶剂。总收率39.0～41.7％。
This article mainly introduces the one-step esterification reaction in the synthesis of 17α-ethynylestradiol, which can improve the reorganization of 3,16α-diacetoxy-estra-1,3,5 (10) -triene- Yield, and to ensure the quality of the precursor of acetylene. Rearrangements react with acetylene magnesium bromide to form 17α- and 17β- two stereoisomers. On separation, the acetonide reaction is carried out in the semi-solid state and is refined with ethyl acetate, without isolation by column chromatography , Which not only simplifies the operation, but also saves the solvent. The total yield of 39.0 ~ 41.7%.