HRID1834988
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 19-hydroxy-6-methyl-5-androstene-3,17-dione bis ethylenektal acetate in methanol is hydrogenated with a 10% palladium-on-charcoal catalyst at atmospheric pressure for a period of about 8 hours. After filtration of the catalyst, additional methanol and aqueous hydrochloric acid are added to the filtrate and the solution is heated to its reflux temperature. After about 30 minutes, the solution is poured onto water, and the solid which separates is filtered and air dried. Crystallization of this solid from an ether-hexane solution yields 19-hydroxy-6β-methyl-5α-androstane-3,17-dione acetate.
WORKUP
后处理
- filtrationAfter filtration of the catalyst, additional methanol and aqueous hydrochloric acid
- additionare added to the filtrate
- temperaturethe solution is heated to its
- temperaturereflux temperature
- additionthe solution is poured onto water
- filtrationthe solid which separates is filtered
- customair dried
- customCrystallization of this solid from an ether-hexane solution