HRID1665627

反应详情

EQUATION

反应方程式

HRID 1665627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

Ammonium chloride (325 mg, 6.0 mmol) in water (10 mL) was added to a solution of 2-benzyloxy-5-nitro-pyridine (350 mg, 1.5 mmol) in THF (15 mL) and the resulting mixture stirred at 75° C. for 30 minutes. Iron powder (340 mg, 6 mmol) was then added portion wise and the mixture stirred for 5 hours at 75° C. The reaction mixture was filtered over celite. The filtrate was basified with sodium bicarbonate solution and the product extracted with ethyl acetate. The organics were washed with brine solution, dried over Na2SO4 and concentrated to afford 320 mg (100%) of 6-benzyloxy-pyridin-3-ylamine.

WORKUP

后处理

  1. stirringthe mixture stirred for 5 hours at 75° C
  2. filtrationThe reaction mixture was filtered over celite
  3. extractionthe product extracted with ethyl acetate
  4. washThe organics were washed with brine solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated