Acetic Acid → HCID 178470180, Verbindung

HRID 2257299Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2257299
C([NH:3][C:4](=O)[C:5]([O-:7])=S)C.Cl.[NH2:10][CH2:11][C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=O.[C:20]([O-])(=O)[CH3:21].[Na+].C(O)(=[O:27])C>>[C:14]1([C:12]2[N:3]=[C:4]([C:5]([O:7][CH2:20][CH3:21])=[O:27])[NH:10][CH:11]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

5

Edukt 4

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 2723597Ethanone, 2-amino-1-phenyl-, hydrochloride (1:1)HCID 178465254HCID 178465254, Verbindung

Produkt 1

HCID 178470180HCID 178470180, Verbindung

Versuchsvorschrift

A mixture of 3 g of ethylthiooxamate, 4.25 g of 2-aminoacetophenone hydrochloride and 3.69 g of sodium acetate was dissolved in 20 mL of acetic acid and heated under reflux for 3 hr. The reaction mixture was allowed to cool to room temperature and the acetic acid removed by evaporation under reduced pressure. The residue was basified with aqueous sodium carbonate and extracted with 2×100 mL of ethyl acetate. The combined extracts were washed with 2×100 mL of brine, dried over anhydrous sodium sulfate and the solvent removed under reduced pressure to yield 2.8 g of ethyl 4-phenylimidazole-2-carboxylate as a solid which was used in the next step without further purification or characterization.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 3 hr
  3. customthe acetic acid removed by evaporation under reduced pressure
  4. extractionextracted with 2×100 mL of ethyl acetate
  5. washThe combined extracts were washed with 2×100 mL of brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d7dd7c24b680494a8d75b5c3807a17bb
Quelldatensatz
uspto-grants-1997_08
Patentnummer
US05656762

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