Sodium Sulfite → HCID 67260704, 화합물

HRID 2359041노트

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HRID 2359041 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]2[C:11]([C:12]3[CH:17]=[CH:16][N:15]=[C:14](SC)[N:13]=3)=[CH:10][N:9]([CH:20]([CH3:22])[CH3:21])[N:8]=2)=[CH:4][CH:3]=1.Cl[C:24]1C=CC=C(C(OO)=O)C=1.[S:34]([O-:37])([O-])=[O:35].[Na+].[Na+]>ClCCl>[Cl:1][C:2]1[S:6][C:5]([C:7]2[C:11]([C:12]3[CH:17]=[CH:16][N:15]=[C:14]([S:34]([CH3:24])(=[O:37])=[O:35])[N:13]=3)=[CH:10][N:9]([CH:20]([CH3:21])[CH3:22])[N:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 672607724-[3-(5-chloro-2-thienyl)-1-isopropyl-1H-pyrazol-4-yl]-2-(methylsulfanyl)pyrimidine

생성물 1

HCID 67260704HCID 67260704, 화합물수율 87.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-[3-(5-chloro-2-thienyl)-1-isopropyl-1H-pyrazol-4-yl]-2-(methylsulfanyl)pyrimidine (1 eq, 12 mmol) in 315 mL of dichloromethane was added meta chloroperbenzoic acid 77% (2 eq, 24 mmol). The mixture was stirred at room temperature for 72 h and then quenched with water. Sodium sulfite (2.1 eq, 25 mmol) was added and the layers were separated. The organic layer was then washed twice with a 2M solution of potassium carbonate, dried over MgSO4 filtered and concentrated to afford 4 g of 4-[3-(5-Chloro-2-thienyl)-1-isopropyl-1H-pyrazol-4-yl]-2-(methylsulfonyl)pyrimidine (65% yield) in a 8:2 mixture with the corresponding sulfoxide. The crude material was used in the next step without further purification.

후처리

  1. customquenched with water
  2. customthe layers were separated
  3. washThe organic layer was then washed twice with a 2M solution of potassium carbonate
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c3b96b74e6f44700bd86629531db6446
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685974B2

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