Reaktion #53786

ord-d578a370dc0942399ec5b135fdf01bfd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationAfter several hours the precipitate was filtered off
  2. 2
    Waschenrinsed three times with water
  3. 3
    Sonstigedried
  4. 4
    SonstigeRecrystallization from ethanol

Vorschrift

1-Dodecanesulfonyl chloride (0.3 g, 1.1 mmol) was added to a stirred solution of 5-(5,6-difluoro-1H-indol-2-yl)-2-methoxy-phenyl-amine from Example 3 (0.3 g, 1.11 mmol) in pyridine (3 mL) under an inert atmosphere at room temperature. After approximately 20 hours the mixture was poured into water (30 mL), stirred, and acidified with aqueous HCl. After several hours the precipitate was filtered off, rinsed three times with water, and dried. Recrystallization from ethanol afforded the product (0.25 g), mp 148-149° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858739B2uspto-grants-2005_02