Reaktion #217761
ord-1b865930ef554f46af6702e236808c8f
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigeare placed in a 250 ml flask
- 2Sonstigeequipped with mechanical agitator
- 3TemperaturThe mixture is heated
- 4Temperaturunder reflux for 1.5 hours
- 5Temperaturheated
- 6Temperaturunder reflux for 3 hours
- 7Sonstigeis formed which
- 8Filtrationis filtered off
- 9Waschenwashed with water
- 10Sonstigedried under vacuum
Vorschrift
10 g of methyl 5-cyano-2,4-dioxo-3-azaspiro[5,5]undecane-1-carboxylate and 5 g of NaOH dissolved in 125 ml of 2:1 ethanol/water are placed in a 250 ml flask equipped with mechanical agitator, thermometer and condenser. The mixture is heated under reflux for 1.5 hours, acidified with 5% HCl to pH 2 and heated under reflux for 3 hours. By cooling to 20° C. a precipitate is formed which is filtered off, washed with water and dried under vacuum. 4.7 g of 2,4-dioxo-3-azaspiro[5,5]undecane are obtained.