Reaktion #1869201
ord-2034badeb438445dac16877f59b9ef1e
Reaktionsgleichung
chloroquinolone
DMF
phosphorus tribromide
sodium carbonate
→
solid
10-Bromo-9-chloro-2,3-dihydro-[1,4]dioxino[2,3-f]quinoline
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturcooling for 30 minutes
- 2workup.STIRRINGstirred for a further 2 hours
- 3TemperaturIt was cooled in ice
- 4Sonstigethe solid was collected
- 5Waschenwashed well with water
- 6Sonstigedried in vacuo
Vorschrift
The chloroquinolone (7a) in dry DMF (8 mL) was cooled in ice and phosphorus tribromide (0.7 mL) added drop-wise, and the mixture was stirred, with ice-cooling for 30 minutes then allowed to warm to room temperature and stirred for a further 2 hours. It was cooled in ice and sodium carbonate solution was added and the solid was collected, washed well with water, and dried in vacuo, to afford a pale yellow solid (1.65 g).