반응 #1888867

반응 방정식

2-(2-Methoxy-ethoxy)-ethyl amine

ethanol

4-chloro-1-(3,5-dimethyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidine

isopropyl ether

→

[1-(3,5-Dimethyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidine-4-yl]-[2-(2-methoxy-ethoxy)-ethyl]-amine

수율 56.8%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타connected to a mechanical stirrer
2. 2
   workup.ADDITIONthermometer socket, condenser and addition funnel
3. 3
   기타Reaction mass temperature
4. 4
   온도was raised
5. 5
   온도to reflux
6. 6
   온도Maintained the mass temperature
7. 7
   온도at reflux for 5 hours
8. 8
   기타Reaction mass temperature
9. 9
   온도Maintained the mass temperature at 25-30° C. for 60 min
10. 10
    기타Reaction mass temperature
11. 11
    온도cooled to 0-5° C
12. 12
    온도Maintained the mass temperature at 0-5° C. for 60 min
13. 13
    기타Solid does not formed
14. 14
    workup.DISTILLATIONDistilled off Ethanol completely under vacuum
15. 15
    기타Crude oily mass was obtained
16. 16
    기타Solid was formed
17. 17
    여과Solid was filtered
18. 18
    세척solid was washed with 50.0 ml of isopropyl ether
19. 19
    기타Compound was dried under vacuum at 60-65° C
20. 20
    기타Dry weight of the compound

실험 절차

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.

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