Hydrochloric Acid → HCID 20184547, Verbindung

HRID 1380721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1380721
[CH3:1][N:2]([CH3:21])[C:3]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:4]=1[C:12]1[NH:13][C:14]2[C:15]([N:20]=1)=[N:16][CH:17]=[CH:18][CH:19]=2.[ClH:22].[H][H]>CO.[Pd]>[ClH:22].[ClH:22].[CH3:1][N:2]([CH3:21])[C:3]1[CH:8]=[C:7]([NH2:9])[CH:6]=[CH:5][C:4]=1[C:12]1[NH:13][C:14]2[C:15]([N:20]=1)=[N:16][CH:17]=[CH:18][CH:19]=2

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 132845112-(1H-Imidazo[4,5-b]pyridin-2-yl)-N,N-dimethyl-5-nitroanilineHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 20184547HCID 20184547, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

An amount of 2.83 gm of 2-(2'-dimethylamino-4'-nitrophenyl)-imidazo[4,5-b]pyridine was hydrogenated in a mixture of 100 ml of methanol, 10 ml of concentrated methanolic hydrochloric acid, and 1 gm of palladium/charcoal for 4.5 hours at ambient temperature with hydrogen gas at 5 bar. The catalyst was then removed by filtration, the filtrate was concentrated by evaporation, and the residue was triturated with acetone to form crystals, filtered, and then washed with a mixture of ether and acetone.

Aufarbeitung

  1. customThe catalyst was then removed by filtration
  2. concentrationthe filtrate was concentrated by evaporation
  3. customthe residue was triturated with acetone
  4. customto form crystals
  5. filtrationfiltered
  6. washwashed with a mixture of ether and acetone

Quellen und Nachweise

ORD-Eintrag
ord-0d149e7db7d84c7b8b89c3fcf3eed068
Quelldatensatz
uspto-grants-1986_04
Patentnummer
US04582837

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