Reaktion #9812

ord-5cb6d0f152d044ee8dc9a054a97d110f

Lösungsmittel

Reaktionsbedingungen

Temperatur
89°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe carbamoylation reaction
  2. 2
    Temperaturthe mixture was heated to 55–60° C.
  3. 3
    TemperaturThe reaction mixture was warmed
  4. 4
    Sonstigepurified as in Example 1

Vorschrift

The carbamoylation reaction was performed as in Example 1. After about 7–8 hours of stirring the carbamoylation reaction mixture (containing pyridinium bromide, 10-methoxy-5H-dibenz[b,f]azepine, water, toluene, and NaOCN) at room temperature (22° C.), the mixture was heated to 55–60° C., and 500 ml of 10% HCl was added drop-wise and carefully. The reaction mixture was warmed to reflux (89° C.) for 3–4 hours, and then worked up and purified as in Example 1. 32.8 g (58% yield) of crude oxcarbazepine was obtained. The crude afforded 24.9 g (44% overall yield) of pure oxcarbazepine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091339B2uspto-grants-2006_08