Reaktion #67788

ord-b149f7c73543424883c0dce7a7930514

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto obtain a homogeneous solution
  2. 2
    workup.STIRRINGstirred for 2 h
  3. 3
    Filtrationthe precipitated solid was filtered
  4. 4
    Waschenwashed with hot methanol

Vorschrift

To a solution of 2-bromo-5-[(2-fluoro-4-iodophenyl)amino]isonicotinic acid (145.0 mg, 0.33 mmol) in N,N-dimethylformamide (1.50 ml), 1,1′-carbonylbis(1H-imidazole) (60 mg, 0.36 mmol) was added, and the mixture was stirred at room temperature for 7 hours to obtain a homogeneous solution. Ammonium acetate (65 mg, 0.83 mmol) was added, and stirred for 2 h. Water (10 ml) was added, and the precipitated solid was filtered, washed with hot methanol to obtain 2-Bromo-5-(2-fluoro-4-iodo-phenylamino)-isonicotinamide as an yellow solid (85 mg, 58%) LC/MS: [9.59 min; 436, 438]

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524911B2uspto-grants-2013_09