反应详情

A solution of 9-fluoro-11β-hydroxyandrosta-1,4-diene-3,17-dione (2.0 g) in a mixture of acetic anhydride (20 ml) and acetic acid (10 ml) containing p-toluenesulfonic acid (200 mg) is kept at room temperature for 40 hours. Sodium acetate (1.0 g) is added and the mixture is evaporated in vacuo. The residue is diluted with water and extracted with chloroform. The chloroform extracts are combined, washed with a dilute sodium bicarbonate solution and water, dried, evaporated and the residue is chromatographed on a column of silica gel to afford the title compound (1.6 g), melting point 229°-230° C.

1. customthe mixture is evaporated in vacuo
2. additionThe residue is diluted with water
3. extractionextracted with chloroform
4. washwashed with a dilute sodium bicarbonate solution and water
5. customdried
6. customevaporated
7. customthe residue is chromatographed on a column of silica gel