HCID 18953543, Verbindung → 4-(1H-imidazol-1-yl)pyridin-3-amine

HRID 1491636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1491636
[N:1]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[N+:12]([O-])=O)[CH:5]=[CH:4][N:3]=[CH:2]1.[H][H]>C(O)C.[C].[Pd]>[NH2:12][C:7]1[CH:8]=[N:9][CH:10]=[CH:11][C:6]=1[N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1

Komponenten

5

Edukt 2

HCID 18953543HCID 18953543, VerbindungHCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 189535484-(1H-imidazol-1-yl)pyridin-3-amineAusbeute 91,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

4-(1-Imidazolyl)-3-nitropyridine (2.10 g, 11.0 mmol) was dissolved in 20 ml of ethanol. After the atmosphere was replaced with nitrogen, 0.25 g of 10% palladium-carbon was added thereto. After the atmosphere was replaced with hydrogen, hydrogen addition was conducted with stirring at room temperature for 3 days. Palladium-carbon was removed by filtration and the filtered cake was washed with ethanol. The filtrate and the washings were combined and then concentrated. The residue was purified by silica gel column chromatography [eluent: dichloromethane:methanol=8:1-6:1 (v/v)] to obtain 1.62 g of a light brown solid (yield: 91.6%).

Aufarbeitung

  1. additionwas added
  2. customPalladium-carbon was removed by filtration
  3. washthe filtered cake was washed with ethanol
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography [eluent: dichloromethane:methanol=8:1-6:1 (v/v)]

Quellen und Nachweise

ORD-Eintrag
ord-c9dfc296919e4e01a85f1da252008546
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05371086

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