反应详情

3-amino-2-[(2-hydroxyethyl)amino]benzonitrile (38 g, crude), is dissolved in formic acid (150 ml) and stirred under reflux for 1 hour. The reaction mixture is concentrated to dryness under reduced pressure to give a dark solid. This solid is dissolved in 200 ml of methanol with heating and while still hot, 60 ml of triethylamine is added and reflux for 1 hour. The mixture is concentrated under vacuum and the precipitate is filtered and washed with water then dried to give the desired compound (27 g, 70% from intermediate 11).

1. temperatureunder reflux for 1 hour
2. concentrationThe reaction mixture is concentrated to dryness under reduced pressure
3. customto give a dark solid
4. temperaturewith heating
5. temperaturereflux for 1 hour
6. concentrationThe mixture is concentrated under vacuum
7. filtrationthe precipitate is filtered
8. washwashed with water
9. customthen dried