Potassium Permanganate → HCID 12898485, Verbindung

HRID 1579393Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1579393
[Mn]([O-])(=O)(=O)=[O:2].[K+].[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]2[CH2:13][C:14]3[CH:20]=[C:19]([CH:21]([OH:25])[CH:22]([CH3:24])[CH3:23])[CH:18]=[CH:17][C:15]=3[O:16][C:8]=12>CC(C)=O>[C:21]([C:19]1[CH:18]=[CH:17][C:15]2[O:16][C:8]3=[N:7][CH:12]=[CH:11][CH:10]=[C:9]3[C:13](=[O:2])[C:14]=2[CH:20]=1)(=[O:25])[CH:22]([CH3:23])[CH3:24]

Komponenten

4

Edukt 2

HCID 516875Potassium PermanganateHCID 21568412HCID 21568412, Verbindung

Produkt 1

HCID 12898485HCID 12898485, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

11 g of potassium permanganate is added in small portions to a solution of 6 g of 1-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-methyl-1 -propanol in 160 ml of acetone, and the mixture is stirred at 20°C for 3 hours. The reaction mixture is filtered, and the residue is washed thoroughly with chloroform. The filtrate and washings are concentrated, and the residue is purified by column chromatography on silica gel with chloroform as eluent, and further by recrystallization from acetone to give 7-isobutyryl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine melting at 155°-156°C.

Aufarbeitung

  1. filtrationThe reaction mixture is filtered
  2. washthe residue is washed thoroughly with chloroform
  3. concentrationThe filtrate and washings are concentrated
  4. customthe residue is purified by column chromatography on silica gel with chloroform as eluent
  5. customfurther by recrystallization from acetone

Quellen und Nachweise

ORD-Eintrag
ord-1f91f159dfe543b1ab0078d1a403e94a
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03931199

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