HRID358868

反应详情

EQUATION

反应方程式

HRID 358868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.62 g (0.025 mole) of potassium phthalimide were added to a solution of 5.41 g (0.024 mole) of 4-methoxy-2,3,5,6-tetrafluoro-1-nitrobenzene (XXXIII) in 100 ml of dimethylformamide, and the mixture was stirred at room temperature for 3 hours. At the end of this time, the solvent was removed by evaporation under reduced pressure, the residue was dissolved in toluene, and the solution was washed with water, dried and concentrated by evaporation under reduced pressure to give an oily substance. This oily substance was subjected to silica gel column chromatography eluted with toluene, to afford 5.07 g of 4-methoxy-2-phthalimido-3,5,6-trifluoro-1-nitrobenzene (XXXIV) as pale yellow powdery crystals.

WORKUP

后处理

  1. customAt the end of this time, the solvent was removed by evaporation under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. washthe solution was washed with water
  4. customdried
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customto give an oily substance
  7. washeluted with toluene