反应详情

A solution of 20 g of 9-fluoro-11β-hydroxyandrosta-1,4-diene-3,17-dione, 120 ml of glacial acetic acid, 120 ml of acetic anhydride and 5 g of p-toluenesulfonic acid is stirred at room temperature under nitrogen for 24 hours. The resulting solution is quenched with 5 g of sodium acetate. The solvent is partially removed in vacuo at 35°-40° C. and the resultant slurry is diluted with chloroform. The chloroform solution is washed with water, saturated sodium bicarbonate and water, dried over anhydrous Na2SO4 and evaporated in vacuo to give the title compound. This is crystallized from ethyl acetate-hexane to give 20 g of the title compound melting point 171°-174° C., with consistent spectral data.

1. customThe resulting solution is quenched with 5 g of sodium acetate
2. customThe solvent is partially removed in vacuo at 35°-40° C.
3. additionthe resultant slurry is diluted with chloroform
4. washThe chloroform solution is washed with water, saturated sodium bicarbonate and water
5. dry with materialdried over anhydrous Na2SO4
6. customevaporated in vacuo