HRID897910

反应详情

EQUATION

反应方程式

HRID 897910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a mixture of 2-nitro-4-(trifluoromethoxy)phenol (2 g, 0.0089 mol) in ethanol (50 mL) and water (25 mL) was added sodium thiosulfate (6.2 g, 0.0356 mol) at room temperature. The heterogeneous mixture was stirred at 80° C. under an atmosphere of nitrogen for 1 hour. The reaction mixture was cooled to room temperature, and ethanol was removed under reduced pressure. The aqueous layer was extracted with ethyl acetate (3×70 mL), and the organic layer was washed with brine and dried under sodium sulfate. The solvent was removed under reduced pressure to give yellow solid of 2-amino-4-(trifluoromethoxy)phenol (0.9 g, 0.005 mol). TLC (methanol/dichloromethane=5:95) Rf 0.29 MS: MH+: 194.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customethanol was removed under reduced pressure
  3. extractionThe aqueous layer was extracted with ethyl acetate (3×70 mL)
  4. washthe organic layer was washed with brine
  5. customdried under sodium sulfate
  6. customThe solvent was removed under reduced pressure