Reaktion #521875

ord-8828d21d6db64a65995c8db756b60f40

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas reacted at 150° C. for 8 hours
  2. 2
    workup.DISTILLATIONwas distilled off under reduced pressure
  3. 3
    Sonstigethe residue was recrystallized repeatedly from dimethylformamide

Vorschrift

A mixture of 56 g of 9-chloro-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid, 71 g of pyrrolidone and 60 ml of hexamethylphosphoric triamide in a stainless steel autoclave was reacted at 150° C. for 8 hours. After completion of reaction, hexamethylphosphoric triamide was distilled off under reduced pressure and the residue was recrystallized repeatedly from dimethylformamide to give 25 g of 9-(1-pyrrolidinyl)-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid. m.p. not lower than 300° C., pale yellow rhombic crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04399134uspto-grants-1983_08