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
To a solution of (4RS,5SR)-5-(4-fluorophenyl)-4-((4-methyl-3-((1,1,2,2-tetrafluoroethyl)oxy)phenyl)methyl)-1,3-oxazolidin-2-one (2.7 g, 6.73 mmol) in ethanol (10 ml) was added 8N aqueous sodium hydroxide solution (4.2 ml, 33.6 mmol), and the mixture was heated under reflux for 4 hrs. The reaction solution was concentrated, diluted with water (100 ml), and the mixture was extracted with ethyl acetate (100 ml×2). The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The residue-was recrystallized from ethyl acetate-hexane to give (1RS,2SR)-2-amino-1-(4-fluorophenyl)-3-(4-methyl-3-((1,1,2,2-tetrafluoroethyl)oxy)phenyl)-1-propanol (2.25 g, 89%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 4 hrs
- concentrationThe reaction solution was concentrated
- additiondiluted with water (100 ml)
- extractionthe mixture was extracted with ethyl acetate (100 ml×2)
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated under reduced pressure
- customThe residue-was recrystallized from ethyl acetate-hexane