Acetic Anhydride → HCID 10490701, Verbindung

HRID 1488495Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1488495
C(O[C:5](=[O:7])[CH3:6])(=O)C.[N+:8]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][N:18]2[CH:22]=[N:21][N:20]=[CH:19]2)=[CH:13][CH:12]=1)([O-:10])=[O:9]>N1C=CC=CC=1>[C:5]([N:17]([N:18]1[CH:22]=[N:21][N:20]=[CH:19]1)[C:14]1[CH:13]=[CH:12][C:11]([N+:8]([O-:10])=[O:9])=[CH:16][CH:15]=1)(=[O:7])[CH3:6]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 108458884-Nitrophenyl(1,2,4-triazol-4-yl)amine

Produkt 1

HCID 10490701HCID 10490701, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2.8 Milliliters of acetic anhydride was added to 15 ml of a pyridine solution containing 0.62 g of 4-[(4-nitrophenyl)amino]-4H-1,2,4-triazole at room temperature and the mixture was stirred for about 2 hours. After completion of reaction, the solvent was removed by distillation under reduced pressure, and a proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue obtained, which was then extracted several times each with ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography to give 0.52 g of 4-[N-acetyl-N-(4-nitrophenyl)amino]-4H-1,2,4-triazole from the chloroform/methanol (100/1) eluate.

Aufarbeitung

  1. customAfter completion of reaction
  2. customthe solvent was removed by distillation under reduced pressure
  3. additiona proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue
  4. customobtained
  5. extractionwhich was then extracted several times each with ethyl acetate
  6. washThe ethyl acetate layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was removed by distillation under reduced pressure
  9. customThe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c598b818107a4bd88aa68bddeec8282c
Quelldatensatz
uspto-grants-1997_10
Patentnummer
US05674886

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