HRID1860366

反应详情

EQUATION

反应方程式

HRID 1860366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 2-nitro-6(5H)-phenanthridinone (3.8 g, 0.0 16 mol) in DMF (200 mL) was added an ammonium chloride solution (3%, 200 mL), followed by the addition of iron powder (22 g). The reaction mixture was stirred at 100° C. for 1 hr. The residue was removed by filtration, and the filtrate was made acidic by adding dilute HCl (25%, 20 mL). A solid separated from the solution and was filtered and washed thoroughly with cold water to remove acidic impurities. The solid was then dried under vacuum, to give hydrochloride salt of 2-amino-6(5H)-phenanthridinone (3.4 g, 89%).

WORKUP

后处理

  1. customThe residue was removed by filtration
  2. additionby adding dilute HCl (25%, 20 mL)
  3. customA solid separated from the solution
  4. filtrationwas filtered
  5. washwashed thoroughly with cold water
  6. customto remove acidic impurities
  7. customThe solid was then dried under vacuum