Hydrochloric Acid → HCID 20061014, Verbindung

HRID 1828792Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1828792
Br[C:2]1[NH:6][C:5]([CH3:7])=[N:4][C:3]=1[CH:8]=[O:9].C(=O)([O-])O.[Na+].[ClH:15]>>[Cl:15][C:2]1[NH:6][C:5]([CH3:7])=[N:4][C:3]=1[CH:8]=[O:9]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 122374954-bromo-2-methyl-1H-imidazole-5-carbaldehyde

Produkt 1

HCID 20061014HCID 20061014, Verbindung

Versuchsvorschrift

5-Bromo-2-methylimidazole-4-carbaldehyde (400 mg) was dissolved in conc. hydrochloric acid (6 ml), and the mixture was refluxed under heating for 24 hr. Saturated aqueous sodium hydrogencarbonate solution was added under ice-cooling until the mixture assumed weak alkalinity and the mixture was extracted twice with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and then brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. Hexane was added to the residue and the crystals were collected by filtration to give 5-chloro-2-methylimidazole-4-carbaldehyde (222 mg) as yellow crystals.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 24 hr
  3. temperaturecooling until the mixture
  4. extractionthe mixture was extracted twice with ethyl acetate
  5. washThe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. additionHexane was added to the residue
  9. filtrationthe crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-bea49ee2b48a4ce7bebf5cb4c9f0e2f5
Quelldatensatz
uspto-grants-2006_06
Patentnummer
US07060721B1

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