Methanol → 2-Methoxypyridin-4-amine
Reaktionsgleichung
Cl[C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.[CH3:9][OH:10]>>[CH3:9][O:10][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1Komponenten
3
Versuchsvorschrift
Na (0.7 g, 30 mmol) was added to methanol (10 mL) at room temperature. Once all Na had dissolved, 2-chloro-4-aminopyridine (0.5 g, 3.9 mmol) was added. The solution was heated to reflux for 16 hours. After the reaction solution cooled to room, it was partitioned between ethyl acetate and water. The aqueous layer was extracted twice with additional ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered, and concentrated under vacuum to give the title product. MS (DCI) m/e 125 (M+H)+.
Aufarbeitung
- dissolutionOnce all Na had dissolved
- temperatureThe solution was heated
- temperatureto reflux for 16 hours
- temperatureAfter the reaction solution cooled to room, it
- customwas partitioned between ethyl acetate and water
- extractionThe aqueous layer was extracted twice with additional ethyl acetate
- washThe combined organic layers were washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-85070f94ff054c27998d8d260804425f
- Quelldatensatz
- uspto-grants-2008_11
- Patentnummer
- US07456169B2
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