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3,3-(亚乙二氧基)雌甾-5(10),9(11)-二烯-17-酮经乙炔加成,与苯硫氯反应,脱苯亚磺酰基,去甲基重排,羰基保护制得3,3:20,20-二(亚乙二氧基)-17α-羟基-19-去甲孕甾-5(10),9(11)-二烯(7),7以六氟丙酮为催化剂环氧化制得3,3:20,20-二(亚乙二氧基)-17α-羟基-5α,10α-环氧-19-去甲孕甾-9(11)-烯,然后经格氏加成、去保护、乙酰化合成醋酸乌利司他,总收率23.1%,纯度99.8%。优化后工艺生产成本低,生产周期短,操作简便。
The 3, 3- (ethylenedioxy) estrone-5 (10), 9 (11) -dien-17-one is acetylene-added, reacted with phenylthiochloride, debenzynesulfinyl, (10), 9 (11) -diene (7) was prepared by the rearrangement and carbonyl protection of 3,3: 20,20-di (ethylenedioxy) -17α-hydroxy- , 7 hexafluoroacetone catalyst epoxidation to obtain 3,3: 20,20-bis (ethylenedioxy) -17α-hydroxy-5α, 10α-epoxy-19-norpregnone-9 11) -ene, and then Grignard addition, deprotection, acetylation of ulipristal acetate, the total yield of 23.1%, a purity of 99.8%. After the process of optimization of low production costs, short production cycle, easy to operate.