HRID868399

反应详情

EQUATION

反应方程式

HRID 868399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-Methoxy-3-nitrobenzotrifluoride (95 g) in isopropanol (1.0 liter) and water (250 ml) was mixed with concentrated hydrochloric acid (15 ml). Iron powder (180 g) was added and the mixture was heated and stirred under reflux. After 90 minutes the mixture was cooled to 50° C. and filtered. The residue was washed with isopropanol and the combined filtrates evaporated. The residue was dissolved in toluene and the solution dried (MgSO4) and evaporated. The residue was triturated with light petroleum (b.p. 30°-40°) to give the 3-amino-4-methoxybenzotrifluoride as a colourless solid (68 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. washThe residue was washed with isopropanol
  5. customthe combined filtrates evaporated
  6. dissolutionThe residue was dissolved in toluene
  7. dry with materialthe solution dried (MgSO4)
  8. customevaporated
  9. customThe residue was triturated with light petroleum (b.p. 30°-40°)