m-Chloroperbenzoic acid → HCID 178422841, Verbindung

HRID 872042Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 872042
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][C:13]1[N:18]=[C:17]2[NH:19][CH:20]=[CH:21][C:16]2=[CH:15][CH:14]=1>C(OCC)(=O)C.C(=O)([O-])[O-].[K+].[K+]>[CH3:12][C:13]1[N+:18]([O-:9])=[C:17]2[NH:19][CH:20]=[CH:21][C:16]2=[CH:15][CH:14]=1

Komponenten

5

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 114577166-Methyl-1H-pyrrolo[2,3-b]pyridine

Produkt 1

HCID 178422841HCID 178422841, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8857Ethyl AcetateLösungsmittelHCID 11430Potassium CarbonateLösungsmittel

Versuchsvorschrift

65% m-Chloroperbenzoic acid (1374 mg) was added to a solution of 6-methyl-1H-pyrrolo[2,3-b]pyridine (570 mg) in ethyl acetate (20 ml) under ice-cooling and the mixture was stirred at room temperature for 20 minutes. After concentration of the reaction mixture in vacuo, the resulted residue was diluted with 2% aqueous solution of potassium carbonate and extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated in vacuo. The resulted residue was purified with a NH-silica gel column chromatography (eluting solvent: chloroform/methanol=30/1 to 9/1) to give 6-methyl-1H-pyrrolo[2,3-b]pyridin-7-oxide (575 mg) as a colorless powder.

Aufarbeitung

  1. temperaturecooling
  2. extractionextracted with chloroform
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe resulted residue was purified with a NH-silica gel column chromatography (eluting solvent: chloroform/methanol=30/1 to 9/1)

Quellen und Nachweise

ORD-Eintrag
ord-78e521754ff64888ac0b1ac6680e5286
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975252B2

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