Reaktion #554651

ord-79ab2ff40fbf4f85b71afd236327c6fb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThen the solvent is removed in vacuo
  2. 2
    workup.ADDITIONSome toluene is added
  3. 3
    Sonstigeall volatile components are removed in vacuo again
  4. 4
    SonstigeThe crude product is used without further purification
  5. 5
    SonstigeThen the EtOH is removed in vacuo and diluted aq. HCl
  6. 6
    workup.ADDITIONis added
  7. 7
    Sonstigethe resulting precipitate is collected
  8. 8
    Waschenwashed with cold water
  9. 9
    Sonstigedried
  10. 10
    SonstigeThe resulting product is used without further purification

Vorschrift

1.0 g (6.41 mmol) ethyl 2-aminooxazole-4-carboxylate and 9.10 mL (96.3 mmol) Ac2O are stirred at r.t. over the weekend. Then the solvent is removed in vacuo. Some toluene is added and all volatile components are removed in vacuo again. This procedure is repeated three times. The crude product is used without further purification. b) 1.31 g (6.60 mmol) of ethyl 2-acetamidooxazole-4-carboxylate are added to 33 mL EtOH. 0.55 g (13.2 mmol) LiOH are added and the resulting mixture is stirred at r.t. over night. Then the EtOH is removed in vacuo and diluted aq. HCl is added and the resulting precipitate is collected, washed with cold water and dried. The resulting product is used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08623860B2uspto-grants-2014_01