HRID478164

反应详情

EQUATION

反应方程式

HRID 478164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 4-[(3-cyanophenylamino)methyl]-3-nitrobenzoate (5.79 g) was dissolved in 50 ml of ethanol, then 50 ml of purified water, 0.96 g of ammonium chloride and 4.97 g of iron powder were added and the mixture was refluxed under heating for 40 minutes. The reaction solution was filtered through Celite and concentrated in vacuo. Ethyl acetate was added to the resulting residue. The mixture was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, concentrated in vacuo and dried to give 5.71 g of ethyl 3-amino-4-[(3-cyanophenylamino)methyl]benzoate.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 40 minutes
  3. filtrationThe reaction solution was filtered through Celite
  4. concentrationconcentrated in vacuo
  5. additionEthyl acetate was added to the resulting residue
  6. washThe mixture was washed with a saturated aqueous solution of sodium bicarbonate
  7. dry with materiala saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customdried