Reaktion #215813

ord-accee4d048a54ba7a4465482d978d2c0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated on a steam bath for 4 hours
  2. 2
    TemperaturThe mixture was cooled
  3. 3
    Filtrationfiltered
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in IMS
  5. 5
    Sonstigehydrogen chloride gas bubbled through this solution
  6. 6
    workup.ADDITIONEther was added
  7. 7
    Sonstigecrystallisation
  8. 8
    Filtrationthe mixture was filtered

Vorschrift

A mixture of ethyl 7-ethoxy-4-(4-methoxyanilino)-1,8-naphthyridine-3-carboxylate hydrochloride (2.6 g) and 5M sodium hydroxide solution (60 ml) was heated on a steam bath for 4 hours. The mixture was cooled and filtered. The residue was dissolved in IMS and hydrogen chloride gas bubbled through this solution. Ether was added to induce crystallisation and the mixture was filtered to give ethyl 4-[4-methoxyanilino]-7-oxo-7,8-dihydro-1,8-naphthyridine-3-carboxylate 0.3 hydrochloride hemihydrate, m.p. 243°-246° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05464781uspto-grants-1995_11