公开(公告)号：US4474701A

公开(公告)日：1984-10-02

申请号：US474314

申请日：1983-03-10

申请人： Gerhard Teichmuller ,  Joachim Rabe ,  Harry Henkel

发明人： Gerhard Teichmuller ,  Joachim Rabe ,  Harry Henkel

IPC分类号： C07J1/00 ,  C07J41/00

CPC分类号： C07J1/0011 ,  C07J41/0094

摘要： A process is disclosed for the separation of 4-androsten-3,17-dione/1,4-androstadien-3,17-dione mixtures, which are produced, e.g., upon microbiological sterol-side chain decomposition, through conversion of said mixture into a mixture of 17.beta.-cyano-17.alpha.-hydroxy-4-androsten-3-one/17.beta.-cyano-17.alpha.-hydroxy-1,4-androstadien-3-one, from which the difficultly soluble 17.beta.-cyano-17.alpha.-hydroxy-4-androsten-3-one is separated in crystalline form through filtration, and the 17.beta.-cyano-17.alpha.-hydroxy-1,4-androstadiene remaining in the mother liquor is re-split, directly or after extraction with organic solvent, by treatment in alkaline medium, into 1,4-androstadien-3,17-dione, and isolated as such. The separation of the products follows in high yields, and in sufficient purity for further working-up in the synthesis of androstane and pregnane derivatives, as well as estratrienes.

摘要翻译： 公开了用于分离4-雄甾-3,17-二酮/ 1,4-雄甾烯-3,17-二酮混合物的方法，其通过例如微生物甾醇侧链分解产生，通过所述混合物的转化 转化为17β-氰基-17α-羟基-4-雄甾-3-酮/17β-氰基-17α-羟基-1,4-雄甾烯-3-酮的混合物，难溶于17β- 通过过滤将氰基-17α-羟基-4-雄甾-3-酮以结晶形式分离，并将残留在母液中的17β-氰基-17α-羟基-1,4-雄甾二烯直接再分裂 或者用有机溶剂萃取后，通过在碱性介质中处理，形成1,4-雄甾二烯-3,17-二酮，并将其分离。 产物的分离遵循高产率，并且具有足够的纯度用于进一步处理雄甾烷和孕烷衍生物以及雌三烯的合成。