Reaktion #61659
ord-77418d8c43974fee8734f31649c38fcb
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe mixture is refluxed for 30 minutes
- 2FiltrationThe solid is filtered off
- 3Waschenwashed with dioxane
- 4workup.DISSOLUTIONdissolved in 600 mL dichloromethane/methanol (9:1)
- 5WaschenThe solution is washed with sodium hydrogen carbonate solution
- 6Trocknendried with sodium sulphate
- 7Sonstigeevaporated down
- 8Filtrationfiltered
- 9Sonstigedried
Vorschrift
13.0 g (44 mmol) 5-acetyl-7-benzyloxy-3,4-dihydro-1H-quinolin-2-one are suspended in 130 mL dioxane and combined with 15.0 g (66 mmol) of 2,3-dichloro-5,6-dicyanobenzoquinone. The mixture is refluxed for 30 minutes, cooled to ambient temperature and stirred for a further 2 hours. The solid is filtered off, washed with dioxane and dissolved in 600 mL dichloromethane/methanol (9:1). The solution is washed with sodium hydrogen carbonate solution, dried with sodium sulphate and evaporated down. Then the residue is suspended in methanol, filtered and dried.