Reaktion #1607382

ord-3e46d4f9915840feb7bc270d138077c7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter evaporation of the solvent
  2. 2
    SonstigeThe compound precipitated
  3. 3
    Filtrationafter filtration
  4. 4
    Waschenthe solid was washed with water
  5. 5
    Sonstigedried
  6. 6
    SonstigeThe solid was finally triturated in Et2O

Vorschrift

According to Scheme 4 Step 2: A solution of 6-(4-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-5-methylthiazol-2-ylamino)picolinonitrile (0.69 mmol, 277 mg) in TFA (4 mL) was microwaved for 7 minutes at 100° C. After evaporation of the solvent, the resulting residue was neutralized with a saturated solution of Na2CO3. The compound precipitated and after filtration, the solid was washed with water and dried. The solid was finally triturated in Et2O, DCM and MeOH to yield 6-(5-methyl-4-(1H-pyrazol-4-yl)thiazol-2-ylamino)picolinonitrile (90 μmol, 25 mg, 12%) as a beige solid.

Quelle

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