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
- 70 °C
PROCEDURE
实验过程
To (2S,3S)-3-tert-butoxycarbonylamino-1,2-epoxy-4-phenylbutane obtained in the same manner as in Reference Example 2 (2.75 g) was added ethanol (27.5 ml). 6.8% Aqueous citric acid solution (29.5 g) was then added thereto, and the mixture was stirred at 70° C. for 2 hr. After cooling to room temperature, ethanol was removed under reduced pressure. The residue was extracted with ethyl acetate, dried over anhydrous sodium sulfate and concentrated under reduced pressure. Further, a mixed solvent of hexane (2.5 ml) and ethyl acetate (2.5 ml) was added to allow precipitation of the crystals. The crystals were collected by filtration and washed twice with a mixed solvent of hexane/ethyl acetate (1/1). The obtained crystals were dried to give the objective (4S,5R)-4-benzyl-5-hydroxymethyloxazolidin-2-one (1.79 g) in a yield of 80%.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customethanol was removed under reduced pressure
- extractionThe residue was extracted with ethyl acetate
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- additionFurther, a mixed solvent of hexane (2.5 ml) and ethyl acetate (2.5 ml) was added
- customprecipitation of the crystals
- filtrationThe crystals were collected by filtration
- washwashed twice with a mixed solvent of hexane/ethyl acetate (1/1)
- customThe obtained crystals were dried