Reaktion #66512

ord-33c151020d4c47249cbe42f2e9834dab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe aqueous phase was filtered
  2. 2
    Sonstigeto afford a brown solid which
  3. 3
    Sonstigewas recrystallized thrice with DMF/water

Vorschrift

According to Scheme 5 Step 3: A solution of 4-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-2-(pyridin-2-ylamino)thiazol-5-carbonitrile (0.93 mmol, 360 mg) in TFA (3 mL) was microwaved for 5 min at 140° C. The reaction mixture was neutralized with a saturated solution of Na2CO3 (40 mL) and water (50 mL). The aqueous phase was filtered to afford a brown solid which was recrystallized thrice with DMF/water to yield 4-(1H-pyrazol-4-yl)-2-(pyridin-2-ylamino)thiazol-5-carbonitrile (0.24 mmol, 65 mg, 26%) as an off-white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524718B2uspto-grants-2013_09