反应详情

A solution of 20 g of 9-fluoro-11β-hydroxyandrosta-1,4-dien-3,17-dione, 120 ml of glacial acetic acid, 120 ml of acetic anhydride and 5 g of p-toluenesulfonic acid was stirred at room temperature under nitrogen for 20 hours. The resulting solution was quenched with 5 g of sodium acetate. The solvent was partially removed in vacuo at 35°-40° C. and the resultant slurry was diluted with chloroform. The chloroform solution was washed with water, saturated sodium bicarbonate and water, dried over anhydrous sodium sulfate and evaporated in vacuo to give the title compound. This was crystallized from ethyl acetate-hexane to give 20 g of the title compound melting point 177°-178° C.

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