HRID6353

反应详情

EQUATION

反应方程式

HRID 6353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(4-Acetylphenyl)amino-3-nitropyridine hydrochloride (2.0 g, 71.8 mmol) was partitioned between aqueous sodium hydroxide and dichloromethane (3×20 ml). The combined organic phases were washed with water (20 ml) and concentrated under reduced pressure to give a solid. Ethanol (20 ml) was added, and the solution was hydrogenated over 5% palladium on carbon (0.2 g) at 50 p.s.i. (345 kPa) for 3.5 hours. The catalyst was filtered off, and the solvent removed under reduced pressure to give a brown solid, (1.8 g) which was used directly for the next reaction without purification, m.p. 165°-166° C. (after recrystallisation from ethanol).

WORKUP

后处理

  1. washThe combined organic phases were washed with water (20 ml)
  2. concentrationconcentrated under reduced pressure
  3. customto give a solid
  4. filtrationThe catalyst was filtered off
  5. customthe solvent removed under reduced pressure
  6. customto give a brown solid, (1.8 g) which