9-Anthracenecarboxylic acid → Anthracene-9-carbonyl chloride
Reaktionsgleichung
[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[C:15]([OH:17])=O)=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:20])=O>>[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[C:15]([Cl:20])=[O:17])=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1Komponenten
3
Versuchsvorschrift
A mixture of 18.85 g of 9-anthroic acid and 60 ml of thionyl chloride is heated under reflux for 1 hour. The excess thionyl chloride is removed under vacuum (30 mm; 90° bath temperature); 50 ml of toluene is added and the mixture is concentrated again. This operation is repeated once more to give 20.6 g of 9-anthroyl chloride as a very moisture-sensitive, yellow solid.
Aufarbeitung
- temperatureis heated
- temperatureunder reflux for 1 hour
- customThe excess thionyl chloride is removed under vacuum (30 mm; 90° bath temperature)
- addition50 ml of toluene is added
- concentrationthe mixture is concentrated again