Ethanol → 4-Pyrimidinebutanoic acid,2-amino-6-[[3-fluoro-4-(1h-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]amino]-,ethyl ester
Reaktionsgleichung
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:5]=[C:4]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]4[NH:28][CH:29]=[CH:30][C:23]=34)=[C:17]([F:31])[CH:16]=2)[N:3]=1.S(=O)(=O)(O)O.[CH2:37](O)[CH3:38]>>[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][CH2:9][CH2:10][C:11]([O:13][CH2:37][CH3:38])=[O:12])[CH:5]=[C:4]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]4[NH:28][CH:29]=[CH:30][C:23]=34)=[C:17]([F:31])[CH:16]=2)[N:3]=1Komponenten
4
Versuchsvorschrift
396 mg (0.86 mmol) of 4-(2-amino-6-{[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]amino}pyrimidin-4-yl)butyric acid (from example 130) in 20 ml of ethanol are, after addition of 0.10 ml of sulfuric acid, heated under RF for 20 hours. The mixture is concentrated under reduced pressure, dichloromethane and a little methanol are added and the mixture is extracted with sodium bicarbonate solution. The organic phase is dried over sodium sulfate and the solvent is removed under reduced pressure. This gives the title compound.
Aufarbeitung
- temperatureheated under RF for 20 hours
- concentrationThe mixture is concentrated under reduced pressure, dichloromethane
- additiona little methanol are added
- extractionthe mixture is extracted with sodium bicarbonate solution
- dry with materialThe organic phase is dried over sodium sulfate
- customthe solvent is removed under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-b9d51c09c1574cbd9ae871b911f5ec69
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07737153B2
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