Acetic Acid → HCID 73197187, Verbindung

HRID 636725

Reaktionsgleichung

Reaktionsgleichung von HRID 636725
[CH3:1][C:2]([N+:5]([O-:7])=O)([CH3:4])[CH3:3].C(O)(=O)C.[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1>C(O)C.[Zn]>[N:12]1([C:17]2[CH:24]=[CH:23][C:20]([CH:21]=[N+:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[O-:7])=[CH:19][CH:18]=2)[CH:16]=[CH:15][N:14]=[CH:13]1

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 116722-Methyl-2-nitropropaneHCID 7365304-(1H-imidazol-1-yl)benzaldehyde

Produkt 1

HCID 73197187HCID 73197187, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

To a suspension of 1,1-dimethylnitroethane (261.2 mg, 2.53 mmol) and zinc (247.0 mg, 3.78 mmol) in ethanol (3.0 ml) was added acetic acid (451.8 mg, 7.52 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 30 minutes. After cooling the mixture to 5° C. again, 4-(1-imidazolyl)benzaldehyde (216.5 mg, 1.26 mmol) was added dropwise to the mixture while stirring and stirred at room temperature overnight. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (chloroform/methanol=10/1).

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 30 minutes
  2. stirringwhile stirring
  3. stirringstirred at room temperature overnight
  4. filtrationZinc acetate in the mixture was filtered off
  5. concentrationthe filtrate was concentrated
  6. custompurified by silica gel chromatography (chloroform/methanol=10/1)

Quellen und Nachweise

ORD-Eintrag
ord-bda5bfc6fee9495a97edd7e3f247ff2e
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06194461B1

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