反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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 dissolved in 2 ml of methanol and mixed with 23 mg of sodium borohydride. After 1 hour of stirring at room temperature, the solvent is drawn off in a vacuum for the most part, the residue is mixed with common salt solution, extracted 3 times with methylene chloride, dried on magnesium sulfate and concentrated by evaporation in a vacuum. Preparative thin-layer chromatography with methylene chloride/methanol=9/1 as a mobile solvent provides 42 mg of 11β-fluoro-7α-{5-[methyl-(9,9,10,10,10-pentafluoro-decyl)-amino]-pentyl}-estra-1,3,5(10)-triene-3,17β-diol as a foam, [α]D=+44° (c=1.0 in chloroform).
WORKUP
后处理
- additionthe residue is mixed with common salt solution
- extractionextracted 3 times with methylene chloride
- customdried on magnesium sulfate
- concentrationconcentrated by evaporation in a vacuum