HRID1475176

反应详情

EQUATION

反应方程式

HRID 1475176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a toluene solution (350 mL) of N-(4-methoxybutyl)-2-nitroaniline were added 10% Pd/C (K-type, 50% water-containing product, 10.0 g) and toluene (100 mL). The mixture was stirred at 20-30° C. for 3 hr under a hydrogen pressure (0.1 MPa). Under a nitrogen stream, the catalyst was filtered off and the residue was washed with toluene (100 mL). Water in the filtrate was removed by partitioning, magnesium sulfate (25.0 g) was added at 20-30° C., and the mixture was stirred at the same temperature for 30 min. Magnesium sulfate was filtered off and the residue was washed with toluene (100 mL) to give a toluene solution of N-(4-methoxybutyl)-o-phenylenediamine (yield 100%).

WORKUP

后处理

  1. filtrationUnder a nitrogen stream, the catalyst was filtered off
  2. washthe residue was washed with toluene (100 mL)
  3. customWater in the filtrate was removed
  4. customby partitioning
  5. additionmagnesium sulfate (25.0 g) was added at 20-30° C.
  6. stirringthe mixture was stirred at the same temperature for 30 min
  7. filtrationMagnesium sulfate was filtered off
  8. washthe residue was washed with toluene (100 mL)