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发明公开
CN104774233A 3-(亚乙二氧基)-17β-氰基-17α-三甲基硅氧基-雌-5(10)，9(11)-二烯的制备工艺 无效 - 驳回

3-(亚乙二氧基)-17β-氰基-17α-三甲基硅氧基-雌-5(10)，9(11)-二烯的制备工艺
摘要：
本发明提供了3‐(亚乙二氧基)‐17β‐氰基‐17α‐三甲基硅氧基‐雌‐5(10),9(11)‐二烯的制备工艺，包括以下步骤：将反应底物2加入到无水溶剂中，再加入有机碱，4‐N,N‐二甲基吡啶，在缓慢滴加三甲基氯硅烷，在适当温度下反应一段时间后，检测所述反应底物反应完全后，反应混合物经后处理得到3‐(亚乙二氧基)‐17β‐氰基‐17α‐三甲基硅氧基‐雌‐5(10),9(11)‐二烯(1)，反应式为：该工艺具有如下优点：避免使用大量的三甲基氯硅烷，大大缩短了反应时间，且收率高达96%；通过对其重结晶的纯化，使得下一步的反应收率大大提高；条件温和，容易操作，易于放大，适合工业化生产。
摘要（英）：

The present invention provides a 3-(ethylenedioxy)-17beta-cyano-17alpha-trimethylsiloxy-estr-5(10),9(11)-diene preparation process, which comprises: adding a reaction substrate 2 to an anhydrous solvent, adding an organic alkali and 4-N,N-dimethylpyridine, slowly adding trimethyl chlorosilane in a dropwise manner, reacting for a certain time at a suitable temperature, treating the reaction mixture after the reaction substrate completely reacts to obtain the 3-(ethylenedioxy)-17beta-cyano-17alpha-trimethylsiloxy-estr-5(10),9(11)-diene (1), wherein the reaction formula is defined in the instruction. The preparation process has advantages of avoidance of use of a large amount of trimethyl chlorosilane, substantial reaction time reducing, high yield up to 96%, mild condition, easy operation, and east scale-up, and is suitable for industrial production, wherein the purification is performed on the recrystal so as to substantially increase the yield of the next reaction.

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