反应详情

A solution of 260 mg of 11β-fluoro-3-hydroxy-7α-[5-(methyl-amino)-pentyl]-estra-1,3,5(10)-trien-17-one in 3 ml of dimethylformamide is stirred with 180 mg of 9,9,10,10,10-pentafluorodecyltosylate for 1 hour at a bath temperature of 100° C. Then, it is added to semi-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. 92 mg of 11β-fluoro-3-hydroxy-7α-{5-[methyl-(9,9,10,10,10-pentafluoro-decyl)-amino]-pentyl}-estra-1,3,5(10)-trien-17-one is obtained as a foam, [α]D=+48° (c=1.0 in chloroform).

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