Reaktion #2069083

Reaktionsgleichung

7-Amino-8,9-difluoro-2-methyl-6-oxo-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

piperidine

→

7-amino-8-fluoro-2-methyl-6-oxo-9-(1-piperidyl)-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

Ausbeute 48.7%

Lösungsmittel

N-methylpyrrolidone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture is heated at 110°-120° C. for 5 hours in a sealed tube
2. 2
   EinengenThe reaction mixture is concentrated to dryness under reduced pressure
3. 3
   workup.ADDITIONto the residue is added ethyl acetate
4. 4
   SonstigeThe resulting crystals are separated by filtration
5. 5
   Sonstigerecrystallized from N,N-dimethylformamide

Vorschrift

7-Amino-8,9-difluoro-2-methyl-6-oxo-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (0.5 g) and piperidine (0.8 g) are suspended in N-methylpyrrolidone (10 ml), and the mixture is heated at 110°-120° C. for 5 hours in a sealed tube. The reaction mixture is concentrated to dryness under reduced pressure, and to the residue is added ethyl acetate. The resulting crystals are separated by filtration and recrystallized from N,N-dimethylformamide to give 7-amino-8-fluoro-2-methyl-6-oxo-9-(1-piperidyl)-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (0.3 g) as yellow cubic crystals. m.p. 273°-276° C. (decomp.)

Quelle