Reaktion #7716

ord-bc09a3a13dce4855b85b4efddef0a94f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis evaporated
  2. 2
    SonstigeThe residue is partitioned between DCM and aqueous saturated NaHCO3
  3. 3
    WaschenThe organic layer is washed with brine
  4. 4
    Sonstigedried
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigeevaporated
  7. 7
    SonstigeThe residue is triturated in MeOH
  8. 8
    Filtrationthe resulting white solid is collected by filtration

Vorschrift

To a suspension of the above-prepared [2-methylsulfanyl-6-(morpholin-4-yl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine (500 mg, 1.63 mmol) in MeOH (10 mL) is added a solution of oxone (3.0 g) in water (10 mL). The reaction mixture is stirred at room temperature for 15 hours and most of the solvent is evaporated. The residue is partitioned between DCM and aqueous saturated NaHCO3. The organic layer is washed with brine, dried, filtered and evaporated. The residue is triturated in MeOH and the resulting white solid is collected by filtration to give [2-methylsulfonyl-6-(morpholin-4-yl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087603B2uspto-grants-2006_08