Reaktion #217761

ord-1b865930ef554f46af6702e236808c8f

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeare placed in a 250 ml flask
  2. 2
    Sonstigeequipped with mechanical agitator
  3. 3
    TemperaturThe mixture is heated
  4. 4
    Temperaturunder reflux for 1.5 hours
  5. 5
    Temperaturheated
  6. 6
    Temperaturunder reflux for 3 hours
  7. 7
    Sonstigeis formed which
  8. 8
    Filtrationis filtered off
  9. 9
    Waschenwashed with water
  10. 10
    Sonstigedried 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07381823B2uspto-grants-2008_06