反应详情

Dissolve dl-3-methoxyestra-2,5(10)-dien-17β-ol (4 g) in cyclohexanone (40 ml) and toluene (140 ml) and add a solution of aluminum isopropoxide (4 g) in toluene (56 ml). Reflux in an atmosphere of nitrogen for two hours and cool. Add water (7.5 ml), shake, and then dry by adding sodium sulfate (10 g). Filter and evaporate under vacuum and recrystallize the residue from methanol to obtain dl-3-methoxyestra-2,5(10)-dien-17-one (3.5 g); m.p. 116°-118°; infrared absorption maxima at 5.76 μ, 5.9 μ, 6.01 μ.

1. temperatureReflux in an atmosphere of nitrogen for two hours
2. temperaturecool
3. dry with materialAdd water (7.5 ml), shake, and then dry
4. additionby adding sodium sulfate (10 g)
5. filtrationFilter
6. customevaporate under vacuum
7. customrecrystallize the residue from methanol