Reaktion #320751

ord-1a00feb50a23425d8fdfd059c8a2d639

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with CH2Cl2
  2. 2
    ExtraktionThe organic extract
  3. 3
    Waschenwas washed with brine
  4. 4
    Trocknendried (MgSO4)
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe residue was triturated with ethyl ether

Vorschrift

Potassium persulfate (3.2 g, 7.0 mmol) in water (75 mL) was added to a solution of 4-(fluorophenyl)-1-(methyl-4-piperidinyl)-5-(2-methylthio-4-pyrimidinyl)imidazole (2.7 g, 7.0 mmol) in glacial AcOH (150 mL). After stirring at ambient temperature for 72 h, the reaction mixture was neutralized by the portion-wise addition of concentrated aqueous NH4OH and extracted with CH2Cl2. The organic extract was washed with brine, dried (MgSO4) and concentrated. The residue was triturated with ethyl ether to afford the title compound as an off-white solid; yield 2.3 g (83%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05593992uspto-grants-1997_01