Reaktion #1605794
ord-5a798cbce38d471eb24362d5ff36d87d
Reaktionsgleichung
8-Quinolinol
meta-chloroperbenzoic acid
→
8-hydroxyquinoline-N-oxide
Ausbeute 81.6%
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeInsoluble matter was removed by filtration
- 2Waschenwas washed with dichloromethane
- 3workup.ADDITIONThe filtrate and the washing were mixed
- 4Einengenconcentrated under reduced pressure
- 5workup.ADDITIONTo the residue, 2% aqueous ammonia (2.1 L) was added
- 6workup.STIRRINGthe mixture was stirred at room temperature overnight
- 7FiltrationThe precipitate was collected by filtration
- 8Waschenwashed with purified water
- 9Sonstigedried under reduced pressure
Vorschrift
8-Quinolinol (351 g, 2.42 mol) was dissolved in dichloromethane (3.5 L) and, under ice-water cooling, meta-chloroperbenzoic acid (675.3 g, 2.74 mol) was added thereto in portions, and the mixture was stirred at room temperature for 2 hours. Insoluble matter was removed by filtration and was washed with dichloromethane. The filtrate and the washing were mixed and concentrated under reduced pressure. To the residue, 2% aqueous ammonia (2.1 L) was added and the mixture was stirred at room temperature overnight. The precipitate was collected by filtration, washed with purified water, and dried under reduced pressure to obtain 8-hydroxyquinoline-N-oxide (318.4 g).