Reaktion #52185

ord-47aeff0440d84a1f8079f3dc0a0f8a27

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe reaction mixture was then stirred at room temperature for 16 hours
  2. 2
    Waschenfinally washed with 1 N hydrochloric acid and water
  3. 3
    TrocknenThe organic phase was dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  5. 5
    SonstigeThe crude product was purified by silica gel column chromatography

Vorschrift

With stirring, a mixture of 1.4 mmol of (R)-3,3-dimethylbut-2-ylamine, 1.4 mmol of triethylamine and 10 ml of dichloromethane was introduced into a mixture of 1.4 mmol of 5,7-dichloro-6-(2,4,6-trifluorophenyl)-1,2,4-triazolo[1,5-a]-pyrimidine in 30 ml of dichloromethane. The reaction mixture was then stirred at room temperature for 16 hours and finally washed with 1 N hydrochloric acid and water. The organic phase was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The crude product was purified by silica gel column chromatography. This gave the title compound in the form of colorless crystals in a yield of 76% (m.p.: 169-171° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06855718B2uspto-grants-2005_02