Reaktion #2018591

ord-2bbfaaeeca27455a9cbc468af86954ed

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 30 min
  2. 2
    workup.DISTILLATIONThen 20 ml of ethanol were distilled off
  3. 3
    workup.ADDITIONwater was added
  4. 4
    Filtrationthe precipitate was filtered off
  5. 5
    workup.ADDITION10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added
  6. 6
    FiltrationAfter dilution with water, the precipitated product was filtered off
  7. 7
    Waschenwashed with water
  8. 8
    Sonstigedried

Vorschrift

1.085 g (5 mmol) of 2-bromo-1-(4-fluoro-phenyl)-ethanone and 405 mg (5 mmol) of sodium thiocyanate in 40 ml of ethanol were heated under reflux for 30 min. Then 20 ml of ethanol were distilled off, water was added, the precipitate was filtered off, 10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added, and the mixture was stirred at 100° C. for 1 h. After dilution with water, the precipitated product was filtered off, washed with water and dried. Yield: 782 mg.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08188291B2uspto-grants-2012_05