Reaktionsgleichung
[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>>[C:1]([C:5]1[CH:9]=[C:8](/[N:10]=[CH:13]/[N:14]([CH3:16])[CH3:15])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2]Komponenten
3
Versuchsvorschrift
A mixture of 3-tert-butyl-1H-pyrazol-5-amine (5 g, 36 mmol, Alfa-aesar) and N,N-dimethylformamide dimethylacetal (153 mL, 1078 mmol, Aldrich) was refluxed overnight. The reaction mixture was then cooled, concentrated under reduced pressure and the residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-5% methanol in dichloromethane) to provide 6.9 g (99%) of the title compound. MS (ESI+) m/z 195 (M+H)+.
Aufarbeitung
- temperaturewas refluxed overnight
- temperatureThe reaction mixture was then cooled
- concentrationconcentrated under reduced pressure
- customthe residue was purified by column chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-c0b873635e024ef7ac056cf6682c5210
- Quelldatensatz
- uspto-grants-2015_11
- Patentnummer
- US09193713B2
Verknüpfte Notizen
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