Sodium Bicarbonate → HCID 69218334, Verbindung

HRID 2251082Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2251082
[CH2:1]([O:3][C:4](=[O:33])[CH:5]=[C:6]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[Cl:32])[C:7]1[N:17]([C:18]2[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:19]=2[F:25])[C:10]2[N:11]=[C:12](SC)[N:13]=[CH:14][C:9]=2[CH:8]=1)[CH3:2].O[O:35][S:36]([O-:38])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+].[C:48]([O-])(O)=O.[Na+]>C1COCC1.CO.O>[CH2:1]([O:3][C:4](=[O:33])[CH:5]=[C:6]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[Cl:32])[C:7]1[N:17]([C:18]2[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:19]=2[F:25])[C:10]2[N:11]=[C:12]([S:36]([CH3:48])(=[O:38])=[O:35])[N:13]=[CH:14][C:9]=2[CH:8]=1)[CH3:2]

Komponenten

7

Edukt 4

HCID 516892Sodium BicarbonateHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 69218825HCID 69218825, Verbindung

Produkt 1

HCID 69218334HCID 69218334, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 21899815MeOH tetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 3-(2-chloro-phenyl)-3-[7-(2,6-difluorophenyl)-2-methylsulfanyl-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-acrylic acid ethyl ester, 13, (0.33 g, 0.68 mmol) in THF/methanol (4 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (1.46 g, 2.38 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 extracted with CHCl3 and the combined organic phases are dried (MgSO4), filtered and concentrated in vacuo to afford 0.31 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 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-07d4e6a3af7b445794844495e44ab6f3
Quelldatensatz
uspto-grants-2008_01
Patentnummer
US07319102B1

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