Reaktion #1607383

ord-aab2c10129b44404856c0bcb318415f5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe precipitate formed
  2. 2
    Sonstigewas recovered
  3. 3
    Waschenwashed with DCM
  4. 4
    ExtraktionThe aqueous phase was extracted with DCM
  5. 5
    Waschenthe organic phase was washed
  6. 6
    TrocknenThe organic phase was dried over MgSO4
  7. 7
    Filtrationwas filtered
  8. 8
    Einengenwas concentrated

Vorschrift

According to Scheme 5 Step 1: A solution of N-(4-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)thiazol-2-yl)pyridin-2-amine (4.20 mmol, 1.53 g) and N-bromosuccinimide (4.40 mmol, 782 mg) in DMF (76 mL) was stirred for 1.5 hour at 50° C. The reaction mixture was diluted with a saturated solution of Na2CO3 and water. The precipitate formed was recovered and washed with DCM. The aqueous phase was extracted with DCM and the organic phase was washed. The organic phase was dried over MgSO4, was filtered and was concentrated to yield with the addition of the precipitate N-(4-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-5-bromothiazol-2-yl)pyridin-2-amine (4.02 mmol, 1.78 g, 96%) as a beige solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09073907B2uspto-grants-2015_07