反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
422 mg of N,N'-carbonyldiimidazole were added, whilst ice-cooling, to a solution of 500 mg of 3-phenoxy-2-hydroxypropylamine in 5 ml of anhydrous dimethylformamide, and the mixture was stirred at room temperature overnight. At the end of this time, the solvent was removed from the reaction mixture by evaporation under reduced pressure, and water was added to the resulting concentrate. The mixture was then extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. The ethyl acetate was removed from the extract by evaporation under reduced pressure, and the resulting residue was purified by silica gel column chromatography, using ethyl acetate as the eluent, to give 490 mg of the title compound, melting at 110° C. to 111° C.
WORKUP
后处理
- customAt the end of this time, the solvent was removed from the reaction mixture by evaporation under reduced pressure, and water
- additionwas added to the resulting
- concentrationconcentrate
- extractionThe mixture was then extracted with ethyl acetate
- washThe extract was washed with an aqueous solution of sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- customThe ethyl acetate was removed from the
- extractionextract by evaporation under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography