反应详情

A mixture of methyl-17β-cyclohexylcarbonyl-estra-1,3,5(10)-triene-3-carboxylate (0.14 g, 0.34 mmol), K2CO3 (0.2 g, 1.45 mmol), water (3.0 mL) and methanol (30 mL) was heated at reflux overnight. The reaction mixture was then concentrated. The residue was diluted with water, acidified with dilute HCl and extracted with ethyl acetate. The organic extract was washed with brine, dried, and concentrated. The resulting solid was washed with CH3CN and isolated by filtration from boiling ethyl acetate to give, 0. 11 g of the title compound. mp 280°-285° C. (softened at 260° C.).

1. temperaturewas heated
2. temperatureat reflux overnight
3. concentrationThe reaction mixture was then concentrated
4. additionThe residue was diluted with water
5. extractionextracted with ethyl acetate
6. extractionThe organic extract
7. washwas washed with brine
8. customdried
9. concentrationconcentrated
10. washThe resulting solid was washed with CH3CN
11. customisolated by filtration
12. customto give