Hydrochloric Acid → N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-aminoisonicotinamide
Reaktionsgleichung
[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH:18]C(=O)C)[CH:13]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].Cl>C(O)C>[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][N:15]=[C:14]([NH2:18])[CH:13]=2)[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 85 °C
Versuchsvorschrift
N4-[4-(tert-Butyl)-1,3-thiazol-2-yl]-2-(acetylamino)isonicotinamide (546 mg) dissolved in ethanol (12 ml) was added dropwise with concentrated hydrochloric acid (1.2 ml) at room temperature and stirred at 80-90° C. for 1 hour. The reaction solution was returned to room temperature, concentrated under reduced pressure, neutralized with 1 N sodium hydroxide and extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (chloroform→chloroform:methanol=60:1→20:1) to obtain 247.2 mg (52%) of the title compound as white crystals.
Aufarbeitung
- customwas returned to room temperature
- concentrationconcentrated under reduced pressure
- extractionextracted with chloroform
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography (chloroform→chloroform:methanol=60:1→20:1)
Quellen und Nachweise
- ORD-Eintrag
- ord-a4174dac4bad4b44b79eb207637c13c5
- Quelldatensatz
- uspto-grants-2006_06
- Patentnummer
- US07056917B2
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