반응 #7716

ord-bc09a3a13dce4855b85b4efddef0a94f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타is evaporated
  2. 2
    기타The residue is partitioned between DCM and aqueous saturated NaHCO3
  3. 3
    세척The organic layer is washed with brine
  4. 4
    기타dried
  5. 5
    여과filtered
  6. 6
    기타evaporated
  7. 7
    기타The residue is triturated in MeOH
  8. 8
    여과the resulting white solid is collected by filtration

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087603B2uspto-grants-2006_08