Reaktion #161869

ord-823ddf6bf1f54c0c800a71b1bba1c675

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThen the reaction mixture was evaporated down
  2. 2
    workup.ADDITIONthe residue was mixed with water
  3. 3
    Filtrationfiltered
  4. 4
    workup.STIRRINGstirred with diisopropylether and isopropanol and suction
  5. 5
    Filtrationfiltered again
  6. 6
    TrocknenAfter drying the crude product
  7. 7
    Sonstigewas purified by preparative HPLC-MS
  8. 8
    Sonstigefreeze-dried

Vorschrift

0.74 g (3.4 mmol) 1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-one, 1.0 g (3.2 mmol) (2,6-dichloro-pyridin-4-yl)-(5-fluoro-2,3-dihydro-indol-1-yl)-methanone and 0.65 mL (3.8 mmol) DIPEA in 10 mL DMF were stirred for 2 h at RT. Then the reaction mixture was evaporated down, the residue was mixed with water and stirred for 30 min at RT. The precipitated solid was suction filtered, stirred with diisopropylether and isopropanol and suction filtered again. After drying the crude product was purified by preparative HPLC-MS. The product-containing fractions were combined and freeze-dried.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829006B2uspto-grants-2014_09