反应详情

To 4-(4-benzyl-4,7-diaza-spiro[2.5]oct-7-yl)-7H-pyrrolo[2,3-d]pyrimidine (intermediate 22) (50 g, 78.36 mmol) in MeOH, was added 10% Pd/C (20 g) and HCOONH4 (98 g, 783.69 mmol) and the reaction mixture was heated to reflux for 30 min. The reaction mixture was filtered through celite bed and washed with MeOH and concentrated under reduced pressure. The crude compound was treated with 50% NaOH solution (200 ml) and stirred for 15 min and solid was obtained by filtration. And the solid was wash with 50 ml of water and dried under vacuum. The crude compound (33 g) in acetone (10 times) was heated to reflux for 30 min. The reaction mixture was cooled and filtered and the solid was washed with acetone to afford the title compound as a solid (29.78 g, 83%).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 30 min
3. filtrationThe reaction mixture was filtered through celite bed
4. washwashed with MeOH
5. concentrationconcentrated under reduced pressure
6. additionThe crude compound was treated with 50% NaOH solution (200 ml)
7. customsolid was obtained by filtration
8. washAnd the solid was wash with 50 ml of water
9. customdried under vacuum
10. temperatureThe crude compound (33 g) in acetone (10 times) was heated
11. temperatureto reflux for 30 min
12. temperatureThe reaction mixture was cooled
13. filtrationfiltered
14. washthe solid was washed with acetone