反应详情

温度

27.5 °C

In a four neck round bottom flask, charged dichloromethane (150 ml), 2-((2R)-2-Hydroxy-3-{[4-(3-oxo-4-morpholinyl)phenyl]amino}propyl)-1H-isoindole-1,3(2H)-dione (15 g), N,N′-dicarbonyldiimidazole (9.22 g), and powdered potassium carbonate (5.24 g) at 25 to 30° C. The obtained reaction mass then stirred for 5 h at 25 to 30° C. Reaction mass then filtered and obtained solid is washed the by dichloromethane. Separated filtrate is concentrated under reduced pressure to obtain residue. Added tetrahydrofuran (30 ml) to residue. The obtained mixture is heated to 40 to 45° C. for 30 minutes followed by cooling to room temperature. Finally obtained solid is filtered off and washed by tetrahydrofuran. Yield 90%

1. customThe obtained reaction mass
2. customReaction mass
3. filtrationthen filtered
4. customobtained solid
5. washis washed the by dichloromethane
6. concentrationSeparated filtrate is concentrated under reduced pressure
7. customto obtain residue
8. temperatureThe obtained mixture is heated to 40 to 45° C. for 30 minutes
9. temperatureby cooling to room temperature
10. filtrationFinally obtained solid is filtered off
11. washwashed by tetrahydrofuran