HRID552837

反应详情

EQUATION

反应方程式

HRID 552837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a mixed solution of 4-hydroxy-3-nitrobenzonitrile (1 g) and NH4Cl (163 mg) in ethanol (20 ml), THF (10 ml), and water (10 ml) were added Celite (5 g) and reduced iron (1.7 g), followed by heating under reflux at 70° C. for 30 min. The reaction solution was cooled to room temperature, diluted with EtOAc (200 ml), and then filtered through celite. The solution was washed with saturated brine, the organic layer was dried over anhydrous MgSO4, and filtered, and the filtrate was concentrated under reduced pressure to obtain 3-amino-4-hydroxybenzonitrile (740 mg) as a pale brown solid.

WORKUP

后处理

  1. temperatureby heating
  2. temperatureThe reaction solution was cooled to room temperature
  3. filtrationfiltered through celite
  4. washThe solution was washed with saturated brine
  5. dry with materialthe organic layer was dried over anhydrous MgSO4
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure