Reaktion #1352494

ord-5f8e1b377ea742c18e2495e1d3ae7d62

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGwith stirring
  2. 2
    SonstigeThe crystallizing product is isolated
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried at 20° C
  5. 5
    SonstigeA pure product is obtained by recrystallization from ethanol (180 ml)

Vorschrift

5 g (38 mmol) anhydrous aluminium chloride is introduced into 50 ml ethane-1,2, -dithiol. A solution of 4.7 g of N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide (10 mmol) in 50 ml of dichloromethane is added at 0° C. The mixture is stirred at 0° C. for 4 hours. 50 ml of 10% hydrochloric acid is added dropwise at from 0 to 10° C. with stirring. The crystallizing product is isolated, washed with water and dried at 20° C. A pure product is obtained by recrystallization from ethanol (180 ml).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06545158B2uspto-grants-2003_04