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出 处:《广州化学》2003年第4期25-29,共5页Guangzhou Chemistry
摘 要:分别以酸性脱羧物和碱性脱羧物为起始原料,经官能团的保护制备甲基诺龙。考察了酸性对保护3位羰基的影响,确定了无水乙醇/石油醚是目标分子重结晶的最佳溶剂体系。考擦了格氏试剂(CH3MgI)和甲基锂(CH3Li)对17位羰基的亲核加成反应,发现用甲基锂试剂反应收率可达86.7% 。The 17-methylnortestosterone has been prepared starting from Estr-4-en- 3,17-dione and Estr-5(10)-en-3,17-dione,through protecting the third carbonyl group. In the meanwhile,the effects of varied acids for protecting third carbonyl group were investigated. Through the trial and error,the mixture of anhydrous alcohol / petroleum benzine is the good solvent of target molecule recrystal. Neucleophilic additional reaction of the seventeenth carbonyl group with Grignard and methyllithium was studied. It was found that the reaction of methyllithium had a good yield of 86.7%.
关 键 词:酸性脱羧物 碱性脱羧物 甲基诺龙 17β-羟基-17α-甲基-雌甾-4-烯-3-酮 甾体 甲基锂 格氏试剂 合成
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