Sodium Bicarbonate → HCID 69218330, 화합물

HRID 2251088노트

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HRID 2251088 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([C:10]1[N:20]([C:21]2[N:22]([CH3:27])[N:23]=[C:24]([CH3:26])[CH:25]=2)[C:13]2[N:14]=[C:15](SC)[N:16]=[CH:17][C:12]=2[CH:11]=1)=[O:9].O[O:29][S:30]([O-:32])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+].[C:42]([O-])(O)=O.[Na+]>C1COCC1.O.CO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([C:10]1[N:20]([C:21]2[N:22]([CH3:27])[N:23]=[C:24]([CH3:26])[CH:25]=2)[C:13]2[N:14]=[C:15]([S:30]([CH3:42])(=[O:32])=[O:29])[N:16]=[CH:17][C:12]=2[CH:11]=1)=[O:9]

참가 물질

8

반응물 4

HCID 516892Sodium BicarbonateHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 59643068HCID 59643068, 화합물

생성물 1

HCID 69218330HCID 69218330, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (2-chloro-phenyl)-[7-(2,5-dimethyl-2H-pyrazol-3-yl)-2-methylsulfanyl-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-methanone, 19, (0.13 g, 0.34 mmol) in THF:methanol (4 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (0.73 g, 1.19 mmol) in H2O (4 mL). After stirring the reaction for 1 hour at room temperature, the solution is poured into aqueous saturated NaHCO3. The aqueous phase is twice extracted with CHCl3 and the combined organic phases are dried (MgSO4), filtered and concentrated in vacuo to afford 0.12 g of the desired product which is used without further purification.

후처리

  1. customthe reaction for 1 hour at room temperature
  2. extractionThe aqueous phase is twice extracted with CHCl3
  3. dry with materialthe combined organic phases are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d74f5962af424888a8e8be64dd967a1e
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319102B1

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