HRID358871

反应详情

EQUATION

反应方程式

HRID 358871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.1 g (0.02 mole) of hydrazine hydrate was added to a suspension of 2.15 g (0.007 mole) of N-(3-methoxy-2,4,5-trifluorophenyl)phthalimide (XXXVI) [prepared as described in Step (F3) above] in 30 ml of ethanol, and the mixture was heated under reflux with stirring for 2 hours. The reaction mixture was cooled to room temperature and then filtered. The filtrate was concentrated by evaporation under reduced pressure, and the residue was dissolved in toluene. The resulting solution was washed with water and dried, and the solvent was then removed by evaporation under reduced pressure to afford 1.06 g of 3-methoxy-2,4,5-trifluoroaniline (XXIII) as pale brown needles.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  5. dissolutionthe residue was dissolved in toluene
  6. washThe resulting solution was washed with water
  7. customdried
  8. customthe solvent was then removed by evaporation under reduced pressure