Reaktion #169710

ord-1a5fd13d81a646e38f0218f04b602ff9

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with AcOEt
  2. 2
    TrocknenThe organic layer was dried over MgSO4
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    SonstigeThe residue was chromatographed on silica gel eluting with Hexane/AcOEt=2/1-1/2
  5. 5
    SonstigeThe product was crystallized from AcOEt/hexane

Vorschrift

A mixture of 3-[4-(1H-pyrazolo[3,4-b]pyridin-1-yl)phenyl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (50 mg) and iodoethane (10.5 μl) was stirred at 50° C. for 30 min, treated with water and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was chromatographed on silica gel eluting with Hexane/AcOEt=2/1-1/2. The product was crystallized from AcOEt/hexane to give 1-ethyl-3-[4-(1H-pyrazolo[3,4-b]pyridin-1-yl)phenyl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (13 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846713B2uspto-grants-2014_09