HRID1610773

反应详情

EQUATION

反应方程式

HRID 1610773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (4RS,5SR)-5-(3-chlorophenyl)-4-[4-(1,1-difluoro-2,2-dimethylpropyl)benzyl]-1,3-oxazolidin-2-one (3.82 g, 9.70 mmol) in ethanol (100 ml) was added 8N aqueous sodium hydroxide solution (6.1 ml, 48.5 mmol), and the mixture was heated under reflux for 4 hrs. After completion of the reaction, ethanol was evaporated under reduced pressure. The residue was diluted with water, and the mixture was extracted with ethyl acetate. The organic layers were combined, washed with saturated brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by recrystallization (hexane-ethyl acetate) to give (1RS,2SR)-2-amino-1-(3-chlorophenyl)-3-[4-(1,1-difluoro-2,2-dimethylpropyl)phenyl]-1-propanol (2.56 g, 72%) to give colorless crystals.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hrs
  3. customwas evaporated under reduced pressure
  4. additionThe residue was diluted with water
  5. extractionthe mixture was extracted with ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by recrystallization (hexane-ethyl acetate)