反应详情

A solution of 1.0 g of 11β-fluoro-3-hydroxy-7α-(5-iodopentyl)-estra-1,3,5(10)-trien-17-one in 10 ml of dimethylformamide is stirred with 0.24 ml of pyrrolidine for 2 hours at a bath temperature of 100° C. Then, it is added to saturated sodium bicarbonate solution, extracted three times with methylene chloride, dried on magnesium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with dichloromethane/methanol/triethylamine. 367 mg of 11β-fluoro-3-hydroxy-7α-(5-pyrrolidin-1-yl-pentyl)-estra-1,3,5(10)-trien-17-one is obtained as a foam.

1. extractionextracted three times with methylene chloride
2. customdried on magnesium sulfate
3. concentrationconcentrated by evaporation in a vacuum
4. customchromatographed on silica gel with dichloromethane/methanol/triethylamine