反应详情

A mixture of methyl 17β-benzoyl-estra-1,3,5(10)-triene-3-carboxylate (60 mg, 0.15 mmol), K2CO3 (60 mg, 0.44 mmol), water (1 mL), and methanol (9 mL) was heated at reflux for 5 h. The volatiles were then removed at reduced pressure and the residue was diluted with water, acidified with dilute aqueous HCl, and extracted with EtOAc. The organic extract was washed with water and brine, dried, and evaporated to dryness. Trituration of the residue with acetone and methanol provided the title compound as a white solid, mp 240°-243° C.

1. temperaturewas heated
2. temperatureat reflux for 5 h
3. customThe volatiles were then removed at reduced pressure
4. additionthe residue was diluted with water
5. extractionextracted with EtOAc
6. extractionThe organic extract
7. washwas washed with water and brine
8. customdried
9. customevaporated to dryness