HRID233467
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
In an apparatus supplied with a drierite drying tube, a solution of 19-nor-testosterone (6) (100 g; 0.365 mole) in acetic anhydride (200 ml), pyridine (32 ml) and acetylchloride (320 ml) was heated at reflux under magnetic stirring, for 3 h and then concentrated to dryness under vacuum. The dry residue was triturated in absolute ethanol, filtered and washed with little portions of absolute ethanol. After drying, 19-nortestosterone acetate 3-enolacetate was obtained as a white powder (121.4 g, yield 93%) mp. 176°-177° C. The structure was confirmed by spectroscopic means.
WORKUP
后处理
- customIn an apparatus supplied with a drierite drying tube
- temperatureat reflux under magnetic stirring, for 3 h
- concentrationconcentrated to dryness under vacuum
- customThe dry residue was triturated in absolute ethanol
- filtrationfiltered
- washwashed with little portions of absolute ethanol
- customAfter drying