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改进了自16α,17α-环氧-5-孕甾烯-3β-醇-20-酮(Ⅰ)經五步反应合成物貭S醋酸酯(Ⅵ)的方法,总收率达到45%理論。对(Ⅲ_b)脱溴一步,提出了应用醋酸銨为緩冲剂,在醇溶液中以較少量的Raney鎳为催化剂,在常压下进行选择性的氫解获得成功。
The method for the synthesis of acenaphthene acetate (Ⅵ) from 16α, 17α-epoxy-5-pregnen-3β-ol-20-one (Ⅰ) through five steps was improved. A step of debromination of (Ⅲ_b) is proposed. The use of ammonium acetate as buffering agent and the selective hydrogenolysis under atmospheric pressure with a small amount of Raney nickel as catalyst in alcohol solution are proposed.