反应详情

In 10 ml of acetone is dissolved 1.16 g of 3,3-dimethylbutyric acid, and 5.0 ml of 2N-NaOH is added, followed by addition of 1.15 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 20 ml of DMF. The mixture is refluxed for 5 hours, and thereafter treated in the same manner as Example 26. The reaction mixture is chromatographed on a silica gel column. Following passage of 200 ml of n-hexanediisopropyl ether (3:7), elution is carried out with a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.76 g of the above-identified compound as a colorless viscous oil.

1. additionis added
2. temperatureThe mixture is refluxed for 5 hours
3. additiontreated in the same manner as Example 26
4. customThe reaction mixture is chromatographed on a silica gel column
5. washpassage of 200 ml of n-hexanediisopropyl ether (3:7), elution
6. additionis carried out with a 1:1 mixture of the same solvents
7. customThe eluate is evaporated under reduced pressure
8. customto remove the solvent