Methanol → (2-methylsulfonyl-6-(morpholin-4-yl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine

HRID 7620

Reaktionsgleichung

Reaktionsgleichung von HRID 7620
CS[C:3]1[N:8]=[C:7]([NH:9][C:10]2[NH:11][N:12]=[C:13]([CH3:15])[CH:14]=2)[CH:6]=[C:5]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[N:4]=1.O[O:23][S:24]([O-:26])=O.[K+].[CH3:28]O>O>[CH3:28][S:24]([C:3]1[N:8]=[C:7]([NH:9][C:10]2[NH:11][N:12]=[C:13]([CH3:15])[CH:14]=2)[CH:6]=[C:5]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[N:4]=1)(=[O:26])=[O:23]

Komponenten

5

Versuchsvorschrift

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.

Aufarbeitung

  1. customis evaporated
  2. customThe residue is partitioned between DCM and aqueous saturated NaHCO3
  3. washThe organic layer is washed with brine
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is triturated in MeOH
  8. filtrationthe resulting white solid is collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-bc09a3a13dce4855b85b4efddef0a94f
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07087603B2

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