3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(1,2,4-triazol-1-yl)pyridine → HCID 15289701, Verbindung

HRID 37501

Reaktionsgleichung

Reaktionsgleichung von HRID 37501
[CH2:1]([O:3][C:4]([C:6]1[C:7]([N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)=[N:8][C:9]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:10]([N+:17]([O-])=O)[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:5])[CH3:2].[H][H]>C(OCC)(=O)C.[Pd]>[NH2:17][C:10]1[C:9]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:8][C:7]([N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)=[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13]

Komponenten

5

Edukt 2

HCID 199355863,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(1,2,4-triazol-1-yl)pyridineHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 15289701HCID 15289701, VerbindungAusbeute 66,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

In 25 ml of ethyl acetate was dissolved 0.35 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-(1,2,4-triazol-1-yl)pyridine, whereto 0.2 g of 10% Pd-C (50% wet) was added. The mixture was stirred in a stream of hydrogen at room temperature for 2.5 hours. After the catalyst was removed by filtration, the filtrate was concentrated. The residue was subjected to silica gel column chromatography (eluent:chloroform/ethyl acetate 4:1), to give 0.215 g of the title compound.

Aufarbeitung

  1. additionwas added
  2. customAfter the catalyst was removed by filtration
  3. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-057550317b2a4307b0a358eb949a2dd9
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420275

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