反应详情

A solution of 33 g of 11β-fluoro-7α-(5-hydroxypentyl)oestr-4-ene-3,17-dione in 330 ml of dichloromethane is treated with 28.9 g of triphenylphosphine and 36.7 g of carbon tetrabromide at −5° C. and stirred for 0.5 hours. Dichloromethane is then added and the mixture is washed with water, saturated sodium hydrogencarbonate solution and sodium chloride solution. The organic phase is dried over sodium sulphate and concentrated in vacuo. The crude product is then chromatographed on silica gel using a hexane-ethyl acetate gradient. 28.5 g of 7α-(5-bromopentyl)-11β-fluorooestr-4-ene-3,17-dione of melting point 75-76° C. are obtained.

1. washthe mixture is washed with water, saturated sodium hydrogencarbonate solution and sodium chloride solution
2. dry with materialThe organic phase is dried over sodium sulphate
3. concentrationconcentrated in vacuo
4. customThe crude product is then chromatographed on silica gel using a hexane-ethyl acetate gradient