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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of (S)-2-amino-2-(pyridin-2-yl)ethanol bis hydrochloride (0.80 g, 5.8 mmol) in water (50 mL) cooled to 0° C. was added potassium hydroxide (2.6 g, 46 mmol) and the reaction stirred at 0° C. for 15 minutes, followed by the addition of THF (100 mL) and the reaction cooled to 0° C. To the reaction was next added bis(trichloromethyl) carbonate (1.7 g, 5.8 mmol) and the reaction stirred at 0° C. for 2 hours. The reaction was diluted with EtOAc (300 mL) and the layers were separated. The organic layer was washed with water (100 mL) and brine (100 mL), dried over MgSO4 and concentrated in vacuo. The crude material was chromatographed using EtOAc as eluent to yield (S)-4-(pyridin-2-yl)oxazolidin-2-one (0.20 g, 21%).
WORKUP
后处理
- temperaturethe reaction cooled to 0° C
- stirringthe reaction stirred at 0° C. for 2 hours
- customthe layers were separated
- washThe organic layer was washed with water (100 mL) and brine (100 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe crude material was chromatographed