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Potassium Carbonate → ethyl (2-formyl-1H-imidazol-1-yl)acetate

HRID 856791
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 856791
[CH:1]([C:3]1[NH:4][CH:5]=[CH:6][N:7]=1)=[O:2].[C:8]([O:11][CH2:12][CH2:13]Br)(=[O:10])[CH3:9].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH:1]([C:3]1[N:4]([CH2:9][C:8]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][N:7]=1)=[O:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 249551H-imidazole-2-carbaldehyde

Produkt 1

HCID 62222097ethyl (2-formyl-1H-imidazol-1-yl)acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 2-formylimidazole (5.16 g), bromoethyl acetate (7.1 ml) and potassium carbonate (11.1 g) in. DMF (50 ml) was stirred for 20 hours at 60° C. The insolubles were removed by filtration, water was added to the mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained residue was separated and purified by column chromatography (ethyl acetate:hexane 1:1), to give ethyl (2-formyl-1H-imidazol-1-yl)acetate (1.10 g) as pale yellow oil.

Aufarbeitung

  1. customThe insolubles were removed by filtration, water
  2. additionwas added to the mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was separated
  8. custompurified by column chromatography (ethyl acetate:hexane 1:1)

Quellen und Nachweise

ORD-Eintrag
ord-68b93a7fe6e043de8a1542c6384c7cbb
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07262185B2

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