HRID393398

反应详情

EQUATION

反应方程式

HRID 393398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling to room temperature
  2. customethanol was removed under reduced pressure
  3. extractionThe residue was extracted with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionFurther, a mixed solvent of hexane (2.5 ml) and ethyl acetate (2.5 ml) was added
  7. customprecipitation of the crystals
  8. filtrationThe crystals were collected by filtration
  9. washwashed twice with a mixed solvent of hexane/ethyl acetate (1/1)
  10. customThe obtained crystals were dried