HRID543580

反应详情

EQUATION

反应方程式

HRID 543580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of isoxazolidine hydrochloride (11.0 g) and chloroform (200 ml), under stirring and ice-cooling, was added (±)-2-[4-(4-trifluoromethylphenoxy)phenoxy]propionyl chloride (34.5 g) and then added dropwise triethylamine (22.2 g). After the completion of addition, the reaction mixture was stirred for further 30 minutes at room temperature, to which water was added to form two layers. The organic layer so separated was washed with 1 N hydrochloric acid and then with 1 N aqueous sodium hydroxide and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(±)-2-[4-(4-trifluoromethylphenoxy)phenoxy]propionyl]isoxazolidine (37.3 g) as a white crystalline solid. After recrystallization from a mixture of n-hexane/acetone, the resulting white crystalline solid showed the melting point of 105°-107° C.

WORKUP

后处理

  1. temperatureice-cooling
  2. additionAfter the completion of addition
  3. additionwas added
  4. customto form two layers
  5. customThe organic layer so separated
  6. washwas washed with 1 N hydrochloric acid
  7. dry with materialwith 1 N aqueous sodium hydroxide and dried over anhydrous sodium sulfate
  8. customRemoval of the solvent
  9. distillationby a distillation in vacuo