Water → HCID 20139720, Verbindung

HRID 4483Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 4483
[OH-].[Na+].[CH2:3]([C:6]1[CH:7]=[C:8]2[C:14](=[O:15])[N:13]([C:16]([CH:21]([CH3:23])[CH3:22])([CH3:20])[C:17]([NH2:19])=[O:18])[C:12](=O)[C:9]2=[N:10][CH:11]=1)[CH2:4][CH3:5].O>C1(C)C=CC=CC=1>[CH:21]([C:16]1([CH3:20])[N:13]2[C:14](=[O:15])[C:8]3[C:9](=[N:10][CH:11]=[C:6]([CH2:3][CH2:4][CH3:5])[CH:7]=3)[C:12]2=[N:19][C:17]1=[O:18])([CH3:23])[CH3:22]

Komponenten

5

Edukt 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 20139714alpha-[3-n-propyl-6H-pyrrolo[3,4-b]pyridine-5,7-dione-6-yl]-alpha-isopropyl-alpha-methyl-acetamide

Produkt 1

HCID 20139720HCID 20139720, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

With the simultaneous addition of 0.5 g of powdered sodium hydroxide, a solution of α-[3-n-propyl-6H-pyrrolo[3,4-b]pyridine-5,7-dione-6-yl]-α-isopropyl-α-methyl-acetamide (m.p.: 82° C.) in 100 ml of toluene is heated under reflux for 2 hours in a water separator. After the reaction solution has cooled, it is filtered through silica gel and the filtrate is washed with ethyl acetate and then concentrated by evaporation. The residue is recrystallised from ethyl acetate/petroleum ether, affording 13.1 g of the title compound which melts at 116° C.

Aufarbeitung

  1. temperatureAfter the reaction solution has cooled
  2. filtrationit is filtered through silica gel
  3. washthe filtrate is washed with ethyl acetate
  4. concentrationconcentrated by evaporation
  5. customThe residue is recrystallised from ethyl acetate/petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-a5f8cf3706fb4e88af4fdf400f66f3e5
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04726838

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