反应详情

A solution of 466 mg of 7α-(5-bromopentyl)-11β-fluorooestra-1,3,5(10)-triene-3,17-diol in 10 ml of 1-methyl-2-pyrrolidinone is stirred at a bath temperature of 80° C. for 3 hours with 1.0 g of methyl-(7,7,8,8,9,9,10,10,10-nonafluorodecyl)amine. For work-up, the mixture is added to saturated sodium chloride solution, extracted with ether, dried over sodium sulphate, concentrated in vacuo and the residue is chromatographed on silica gel using ethyl acetate/methanol. 546 mg of 11β-fluoro-7α-{5-[methyl-(7,7,8,8,9,9,10,10,10-nonafluorodecyl)amino]pentyl}-oestra-1,3,5(10)triene-3, 17β-diol are obtained as a foam, [α]D=+39° (c=0.5 in CHCl3)

1. extractionextracted with ether
2. dry with materialdried over sodium sulphate
3. concentrationconcentrated in vacuo
4. customthe residue is chromatographed on silica gel