Sodium Bicarbonate → HCID 69218330, Verbindung

HRID 2251088Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2251088
[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]

Komponenten

8

Edukt 4

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

Produkt 1

HCID 69218330HCID 69218330, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-d74f5962af424888a8e8be64dd967a1e
Quelldatensatz
uspto-grants-2008_01
Patentnummer
US07319102B1

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