Hydrochloric Acid → 6-Fluoro-4-iodopyridin-3-ol
Reaktionsgleichung
Cl.[F:2][C:3]1[CH:8]=[C:7]([I:9])[C:6]([O:10]COC)=[CH:5][N:4]=1.C(=O)(O)[O-].[Na+]>C1COCC1>[F:2][C:3]1[N:4]=[CH:5][C:6]([OH:10])=[C:7]([I:9])[CH:8]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
Add HCl (3 M in water, 31 mL, 93.01 mmol) to a solution of 2-fluoro-4-iodo-5-methoxymethoxy-pyridine (3.9 g, 13.78 mmol) in THF (20 mL). Stir the mixture at 60° C. for 3 hours. Cool down the mixture. Adjust the pH to 7 with slow addition of saturated aqueous sodium bicarbonate solution. Extract the solution with ethyl acetate three times. Wash the organic layer with saturated aqueous sodium chloride. Dry the mixture over sodium sulfate. Concentrate the solution in vacuo to afford the title compound (3.2 g, 97.18%) as a yellow solid. MS (EI) m/z 240 [M+1]+.
Aufarbeitung
- temperatureCool down the mixture
- extractionExtract the solution with ethyl acetate three times
- washWash the organic layer with saturated aqueous sodium chloride
- dry with materialDry the mixture over sodium sulfate
- concentrationConcentrate the solution in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-e6a154c882884f59a91a136e5536f1dd
- Quelldatensatz
- uspto-grants-2011_11
- Patentnummer
- US08063212B2
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