Trifluoromethanesulfonic acid → 2,4-Difluoro-3-(7-pyridin-4-yl-2,3-dihydro-pyrazolo[5,1-b]thiazol-6-yl)phenylamine
Reaktionsgleichung
C([N:8](CC1C=CC=CC=1)[C:9]1[CH:14]=[CH:13][C:12]([F:15])=[C:11]([C:16]2[C:23]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=3)=[C:19]3[S:20][CH2:21][CH2:22][N:18]3[N:17]=2)[C:10]=1[F:30])C1C=CC=CC=1.FC(F)(F)S(O)(=O)=O>C1(C)C=CC=CC=1.C(OCC)(=O)C>[F:30][C:10]1[C:11]([C:16]2[C:23]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=3)=[C:19]3[S:20][CH2:21][CH2:22][N:18]3[N:17]=2)=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[NH2:8]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
To dibenzyl-[2,4-difluoro-3-(7-pyridin-4-yl-2,3-dihydro-pyrazolo[5,1-b]thiazol-6-yl)-phenyl]-amine (180 mg, 0.34 mmol) in toluene (2 mL) was added trifluoro-methanesulfonic acid (3.5 mL) in a sealable vial under nitrogen atmosphere. The mixture was stirred under microwave irradiation at 120° C. for ten minutes. The crude was diluted with ethyl acetate and washed with NaHCO3 saturated solution twice. The organic layer was dried over anhydrous sodium sulfate, filtered and the solvent was removed under reduced pressure. The product was isolated by column chromatography eluting with ethyl acetate: hexane (1: 1) (115 mg).
Aufarbeitung
- washwashed with NaHCO3 saturated solution twice
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customThe product was isolated by column chromatography
- washeluting with ethyl acetate: hexane (1: 1) (115 mg)
Quellen und Nachweise
- ORD-Eintrag
- ord-b5b48a6b34d74338837d59a9249ec437
- Quelldatensatz
- uspto-grants-2013_09
- Patentnummer
- US08524707B2
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