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
- 25 °C
PROCEDURE
实验过程
N-carbobenzoxy-3-fluoro-4-morpholinylaniline (0.33 g, 1 mmol) was added under nitrogen atmosphere to 5 mL of DMF (N,N-dimethyl formamide), and mixture was cooled to −10˜0° C. A solution of lithium tert-butoxide (2.5 mL, 2.5 mmol) in tetrahydrofuran was added dropwise. The mixture was warmed to room temperature (25° C.) naturally and stirred for 2 hours. (S)-1-chloro-3-(dibenzylamino)propan-2-ol (0.32 g, 1.1 mmol) was then added and the mixture was stirred at room temperature for 20 hours. Saturated ammonium chloride solution and ethyl acetate were added to separate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, filtered, and the solvent was evaporated to provide 0.42 g of white solid in 88% yield.
WORKUP
后处理
- temperaturewas cooled to −10˜0° C
- stirringthe mixture was stirred at room temperature for 20 hours
- customto separate
- washThe organic layer was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated