反应详情

To a 500 mL round bottomed flask equipped with a magnetic stir bar, rubber septum, and argon inlet was placed 2 (9 g, 27.8 mmol) and 200 mL of ammonia in methanol (7 N). The mixture was stirred at rt for 24 h. The solution was bubbled with air for 1 h and filtered. The filtrate was acidified with concentrated HCl to pH=2 and concentrated and dried. This solid was again treated with ammonia methanol solution (7 N, 200 mL) for 24 h at rt. The solution was bubbled with air for 1 h and filtered. The filtrate was added concentrated HCl to pH=2 and concentrated. It was filtered and the solid was washed with cooled water and dried to afford compound 3 as a yellow solid (5.2 g, 70%).

1. customTo a 500 mL round bottomed flask equipped with a magnetic stir bar
2. customThe solution was bubbled with air for 1 h
3. filtrationfiltered
4. concentrationconcentrated
5. customdried
6. additionThis solid was again treated with ammonia methanol solution (7 N, 200 mL) for 24 h at rt
7. customThe solution was bubbled with air for 1 h
8. filtrationfiltered
9. additionThe filtrate was added concentrated HCl to pH=2
10. concentrationconcentrated
11. filtrationIt was filtered
12. washthe solid was washed with cooled water
13. customdried