HRID254940

反应详情

EQUATION

反应方程式

HRID 254940 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of morpholin-4-yl-(3-nitro-5-(trifluoromethyl)phenyl)methanone (457 mg, 1.5 mmol) in THF (5 mL) was added dropwise a solution of borane tetrahydrofuran complex solution (3.1 mL, 3.1 mmol) at ambient temperature and the mixture was heated under reflux for 30 minutes, then cooled. The solvent was evaporated. Aqueous HCl (5 mL) was added and the resulting mixture was heated at 100° C. for 1 hour, then cooled and extracted with ether. The acidic aqueous layer was separated, basified to pH 8 with NaOH and extracted with ether. The ether solution was dried over anhydrous Na2SO4. Evaporation of ether provided 168 mg (0.57 mmol) of 4-(3-Nitro-5-trifluoromethylbenzyl)morpholine (38%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. temperaturecooled
  4. customThe solvent was evaporated
  5. additionAqueous HCl (5 mL) was added
  6. temperaturecooled
  7. extractionextracted with ether
  8. customThe acidic aqueous layer was separated
  9. extractionextracted with ether
  10. dry with materialThe ether solution was dried over anhydrous Na2SO4
  11. customEvaporation of ether