反应详情

温度

27.5 °C

60.0 ml of ethanol and 10.0 g (0.038 mol) of 4-chloro-1-(3,5-dimethyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidine (Compound No. 79) were charged into a 250 ml of 4 necked round bottom flask connected to a mechanical stirrer, thermometer socket, condenser and addition funnel. 22.40 g (0.18 mol) of 2-(2-Methoxy-ethoxy)-ethyl amine was charged at 25-30° C. under stirring. Reaction mass temperature was raised to reflux. Maintained the mass temperature at reflux for 5 hours. Reaction mass temperature was cooled to 25-30° C. Maintained the mass temperature at 25-30° C. for 60 min. Reaction mass temperature cooled to 0-5° C. Maintained the mass temperature at 0-5° C. for 60 min. Solid does not formed. Distilled off Ethanol completely under vacuum. Crude oily mass was obtained. Oily mass was dissolved in 45 ml of acetonitrile. 300.0 ml of isopropyl ether was added. Solid was formed. Solid was filtered and solid was washed with 50.0 ml of isopropyl ether. Compound was dried under vacuum at 60-65° C. Dry weight of the compound: 7.50 g (yield—56.80%). Melting point: 90.4° C.

1. customconnected to a mechanical stirrer
2. additionthermometer socket, condenser and addition funnel
3. customReaction mass temperature
4. temperaturewas raised
5. temperatureto reflux
6. temperatureMaintained the mass temperature
7. temperatureat reflux for 5 hours
8. customReaction mass temperature
9. temperatureMaintained the mass temperature at 25-30° C. for 60 min
10. customReaction mass temperature
11. temperaturecooled to 0-5° C
12. temperatureMaintained the mass temperature at 0-5° C. for 60 min
13. customSolid does not formed
14. distillationDistilled off Ethanol completely under vacuum
15. customCrude oily mass was obtained
16. customSolid was formed
17. filtrationSolid was filtered
18. washsolid was washed with 50.0 ml of isopropyl ether
19. customCompound was dried under vacuum at 60-65° C
20. customDry weight of the compound