Reaktion #44697
ord-63c7feb226134404a5bf0269df3955a5
Reaktionsgleichung
2,6-difluorobenzonitrile
potassium carbonate
3-chloro-4-hydroxyaniline
→
2-(4-Amino-2-chlorophenoxy)-6-fluorobenzonitrile
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturthe mixture is heated
- 2Temperaturat reflux for 45 min
- 3FiltrationThe mixture is filtered
- 4Waschenthe filtercake is washed with ethyl acetate and DCM
- 5SonstigeThe solvent is removed under reduced pressure
Vorschrift
1.00 g (7.19 mmol) of 2,6-difluorobenzonitrile is initially charged in 10 ml of acetonitrile. 1.99 g (14.4 mmol) of potassium carbonate and 1.03 g (7.19 mmol) of 3-chloro-4-hydroxyaniline are added, and the mixture is heated at reflux for 45 min. The mixture is filtered and the filtercake is washed with ethyl acetate and DCM. The solvent is removed under reduced pressure and the residue is by column chromatography (silica gel 60, gradient column: mobile phase: DCM:petroleum ether=2:1, then DCM).