HRID1610485
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-(phenyloxy)phenyl)-4-((3-((1,1,2,2-tetrafluoroethyl)oxy)phenyl)methyl)-1,3-oxazolidin-2-one (3.7 g, 8.02 mmol) in ethanol (10 ml) was added 8N aqueous sodium hydroxide solution (5.0 ml, 40 mmol), and the mixture was heated under reflux for 4 hrs. The reaction solution was concentrated, diluted with water (100 ml) and extracted with ethyl acetate (100 ml×2). The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. Recrystallization of the residue from ethyl acetate-hexane gave (1RS,2SR)-2-amino-1-(4-(phenyloxy)phenyl)-3-(3-((1,1,2,2-tetrafluoroethyl)oxy)phenyl)-1-propanol (3.05 g, 87%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 4 hrs
- concentrationThe reaction solution was concentrated
- additiondiluted with water (100 ml)
- extractionextracted with ethyl acetate (100 ml×2)
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated under reduced pressure
- customRecrystallization of the residue from ethyl acetate-hexane