HRID1610476
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)-4-((4-fluorophenyl)methyl)-5-(4-(trifluoromethyl)phenyl)-1,3-oxazolidin-2-one (18 g, 53.1 mmol) in ethanol (300 ml) was added 8N aqueous sodium hydroxide solution (19.9 ml, 159 mmol), and the mixture was heated under reflux for 4 hrs. The reaction solution was concentrated, diluted with water (300 ml), and extracted with ethyl acetate (300 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-3-(4-fluorophenyl)-1-(4-(trifluoromethyl)phenyl)-1-propanol (14.1 g, 85%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 4 hrs
- concentrationThe reaction solution was concentrated
- additiondiluted with water (300 ml)
- extractionextracted with ethyl acetate (300 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