Reaktion #699661

ord-0400c73362384427be9c7378d34ea783

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux, for 5 hrs
  2. 2
    TemperaturThe mixture was cooled to approximately 10° C.
  3. 3
    Filtrationfiltered
  4. 4
    WaschenThe filter cake was washed with cold water
  5. 5
    Sonstigedried under vacuum at 80° C.

Vorschrift

A solution of 2,3-dihydro-4-fluoro-5-methoxy-N-(4-pyridinyl)-1H-isoindol-2-amine (3.25 g) in 48% hydrobromic acid (25 ml) was stirred, under reflux, for 5 hrs. The reaction mixture was diluted with water and stirred at ambient temperature overnight. The mixture was cooled to approximately 10° C. and filtered. The filter cake was washed with cold water and dried under vacuum at 80° C. to give 2.8 g (69%) of product. Recrystallization from water gave the analytical sample, mp. >250° C., dried at 80° C. under vacuum.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06004977uspto-grants-1999_12