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

HRID 7620

반응식

HRID 7620 반응식
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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 23707502Potassium hydroxy sulfiteHCID 178419055[2-methylsulfanyl-6-(morpholin-4-yl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine

생성물 1

HCID 178419103(2-methylsulfonyl-6-(morpholin-4-yl)-pyrimidin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine

시약·촉매·용매 1

HCID 962Water용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc09a3a13dce4855b85b4efddef0a94f
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087603B2

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