反应详情

A solution of 78.7 g of 11β-fluoro-7α-(5-hydroxypentyl)-estr-4-ene-3,17-dione (Example 12e) in 1.41 of carbon tetrachloride and 475 ml of acetonitrile is stirred with 71 g of triphenylphosphine for 8.5 hours at room temperature. Then, it is extracted with water, aqueous sodium bicarbonate and common salt solution, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with hexane/ethyl acetate. 48.0 g of 7α-(5-chloropentyl)-11β-fluoro-estr-4-ene-3,17-dione is obtained as crystals with a melting point of 51-53° C. [α]D22 =+78.5° (c=0.5% in chloroform).

1. extractionThen, it is extracted with water, aqueous sodium bicarbonate and common salt solution
2. customdried on sodium sulfate
3. concentrationconcentrated by evaporation in a vacuum
4. customchromatographed on silica gel with hexane/ethyl acetate