HRID1860366
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe residue was removed by filtration
- additionby adding dilute HCl (25%, 20 mL)
- customA solid separated from the solution
- filtrationwas filtered
- washwashed thoroughly with cold water
- customto remove acidic impurities
- customThe solid was then dried under vacuum