醋酸妊娠双烯醇酮肟的工艺研究

Synthesis Process Study of 16-dehydropregnenolone Acetate Oxime

醋酸妊娠双烯醇酮肟是多个甾体激素合成的中间体,如去氢表雄酮,癸酸诺龙,炔诺酮等。原工艺中使用到吡啶来进行肟化反应,对环境和人员有较大影响。通过实验,进行了吡啶的替代工艺研究,最终发现醋酸钠水溶液对工艺肟化反应更好,并对醋酸钠的投料量和反应时间进行了最优研究。得出最优化的工艺为用醋酸钠水溶液替代吡啶,醋酸钠与I的质量比为0.5∶1,反应时间为50～60℃反应1 h后,回流反应2 h。实现了工艺绿色化,并且收率有明显提高。

The 16-dehydropregnenolone acetate oxime was a key intermediate to systhesis many steroids products,such as dehydroepiandrosterone,nandrolone decanoate,and norethisterone.The pyridine,a limited solvent because of the toxicity to operator and the environment,was used in the literature process.Through the experiment research,the sodium acetate water solution was found successfully to replace the pyridine,and the adding quantity and the reaction time have been researched.The optimal process was got using the sodium acetate to replace the pyridine,the quality ratio 0.5：1,react 1 h at 50～60 ℃ and then reflux for 2 h.The green synthesis was realized,and yield was increased obviously.