Ethyl Acetate → HCID 57927460, Verbindung

HRID 889154Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889154
[O:1]1[CH:5]=[C:4]([C:6]([NH:8][NH2:9])=[O:7])[N:3]=[CH:2]1.CCCCCCC.[C:17](OCC)(=[O:19])C>ClC(OC(Cl)(Cl)Cl)=O>[O:1]1[CH:5]=[C:4]([C:6]2[O:7][C:17](=[O:19])[NH:9][N:8]=2)[N:3]=[CH:2]1

Komponenten

5

Edukt 3

HCID 8857Ethyl AcetateHCID 8900HeptaneHCID 497617151,3-Oxazole-4-carbohydrazide

Produkt 1

HCID 57927460HCID 57927460, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10426DiphosgeneLösungsmittel

Versuchsvorschrift

After suspending oxazole-4-carboxylic acid hydrazide (CAS 885274-12-4) (1.06 g) in ethyl acetate (10 ml), trichloromethyl chloroformate (1.21 ml) was added dropwise while stirring on ice. Upon completion of the dropwise addition, the mixture was heated to reflux for 2 hours and 20 minutes. It was then allowed to cool, n-heptane was added to the reaction mixture, and the precipitate was collected by filtration. The filtrate was concentrated under reduced pressure and the residue was recrystallized with toluene-ethyl acetate. This was combined with the previously filtered substance to obtain the title compound (1.38 g).

Aufarbeitung

  1. additionwas added dropwise
  2. additionUpon completion of the dropwise addition
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 2 hours and 20 minutes
  5. temperatureto cool
  6. filtrationthe precipitate was collected by filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue was recrystallized with toluene-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-f410baf8e0504ce09ec5f5587acf8550
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252810B2

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