Reaktion #338555

ord-1ce963fc4d25473b9ef51ec57da92997

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe solution was extracted with ethyl acetate (3 mL ×2)
  2. 2
    WaschenThe organic phase was then washed with water (3 mL)
  3. 3
    Trocknendried over Na2SO4
  4. 4
    Sonstigeevaporated
  5. 5
    SonstigeThe residue was purified by preparative TLC plate

Vorschrift

A solution of 5-amino-1-(5-cyclopropylcarbamoyl-2-methylphenyl)-1H-pyrazole-4-carboxylic acid (21 mg), 2-methylcyclohexylamine (10 mg), EDCI (28 mg) and HOBt (12 mg) in DMF (0.75 ml) was reacted at room temperature for 24 h. Water (4 ml) was added and the solution was extracted with ethyl acetate (3 mL ×2). The organic phase was then washed with water (3 mL), dried over Na2SO4 and evaporated. The residue was purified by preparative TLC plate to give the desired product 5-amino-1-(5-cyclopropylcarbamoyl-2-methylphenyl)-1H-pyrazole-4-carboxylic acid (2-methylcyclohexyl)-amide (19 mg, 70%). HPLC (4 minute gradient) tR 2.34 min; MS m/z 396.31 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07863314B2uspto-grants-2011_01