反应详情

To the crude product (100 g) of 2-hydroxyestradiol 17-acetate obtained by the process described in Example 3-a, MeOH (3600 ml) and concentrated HCl (400 ml) were added, and the solution was refluxed for 1 hour. After the reaction mixture was cooled, water and AcOEt were added to it and the solution was neutralized by addition of NaHCO3, and extracted with AcOEt. The organic layer was washed with brine, and dried over anhydrous Na2SO4, and then evaporated in vacuo to obtain a crude product (68.7 g), which was, in turn, subjected to silica gel chromatography (elution solvent, hexane:AcOEt=1:1) to afford 59 g (91% from 2-acetylestradiol 17-acetate) of the titled compound.

1. additionwere added
2. temperaturethe solution was refluxed for 1 hour
3. temperatureAfter the reaction mixture was cooled
4. extractionextracted with AcOEt
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous Na2SO4
7. customevaporated in vacuo
8. customto obtain a crude product (68.7 g), which
9. washsubjected to silica gel chromatography (elution solvent, hexane:AcOEt=1:1)