Reaktion #706467

Reaktionsgleichung

1,6-Difluoronaphthalene

Aluminum trichloride

Acetic anhydride

→

1-(4,7-difluoronaphth-1-yl)-ethanone

Ausbeute 80.0%

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining a temperature of 0° C
2. 2
   workup.ADDITIONThe reaction was poured onto ice-cold 10% aqueous hydrochloric acid
3. 3
   Extraktionextracted with methylene chloride (2×10 mL)
4. 4
   TrocknenThe organic layer was dried over sodium sulfate
5. 5
   Einengenconcentrated
6. 6
   Sonstigepurified by column chromatography

Vorschrift

1,6-Difluoronaphthalene (0.164 g, 1.0 mmol) was dissolved in 1,2-dichloroethane (5 mL) and cooled to 0° C. Aluminum trichloride (0.264 g, 2.0 mmol) was added as a solid to the solution. Acetic anhydride (0.1 mL, 1.0 mmol) was added slowly over 20 minutes to the solution while maintaining a temperature of 0° C. The reaction was poured onto ice-cold 10% aqueous hydrochloric acid and extracted with methylene chloride (2×10 mL). The organic layer was dried over sodium sulfate, concentrated, and purified by column chromatography to give 1-(4,7-difluoronaphth-1-yl)-ethanone as an oil (0.165 g, 80%).

Quelle