反应 #499130

反应方程式

4-[(3,4-dichloro-6-fluorophenyl)amino]-6-nitroquinazoline

ethanol

water

hydrazine hydrate

hydrazine hydrate

→

compound 2

4-[(3,4-dichloro-6-fluorophenyl)amino]-6-aminoquinazoline

溶剂

iso-propylalcohol

反应条件

后处理

1. 1
   温度to reflux temperature
2. 2
   温度the reflux was maintained for 20 minutes
3. 3
   过滤Filtration, evaporation and silica gel chromatography (using 90% CH2Cl2/10% MeOH as elute)

实验过程

A solution of 4-[(3,4-dichloro-6-fluorophenyl)amino]-6-nitroquinazoline (1.09 mmol) in 18 ml 9:1 ethanol:water and 11 ml iso-propylalcohol was heated to reflux temperature. 250 μl hydrazine hydrate and 0.5 ml Raney®Nickel (in water) were added thereafter. After 30 minutes, additional 50 μl of hydrazine hydrate was added, and the reflux was maintained for 20 minutes. Filtration, evaporation and silica gel chromatography (using 90% CH2Cl2/10% MeOH as elute) gave 4-[(3,4-dichloro-6-fluorophenyl)amino]-6-aminoquinazoline (compound 2) in 75% yield.

来源