Reaktion #2069080

Reaktionsgleichung

8,9-Difluoro-2-methyl-7-nitro-6-oxo-1,2-dihyro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

→

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

Ausbeute 49.8%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the reaction
2. 2
   Filtrationthe cartalyst is filtered off
3. 3
   workup.DISTILLATIONfurther dimethylformamide is distilled off
4. 4
   workup.ADDITIONto the residue is added ethanol
5. 5
   SonstigeThe resulting precipited crystals are separated by filtration
6. 6
   Sonstigerecrystallized from dimethylformamide

Vorschrift

8,9-Difluoro-2-methyl-7-nitro-6-oxo-1,2-dihyro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (6 g) is dissolved in dimethylformamide (300 ml) and thereto is added 20% palladium-carbon catalyst (0.5 g), and the mixture is subjected to a catalytic reduction under a pressure of 5 kg/cm2. After the reaction, the cartalyst is filtered off and further dimethylformamide is distilled off, and to the residue is added ethanol. The resulting precipited crystals are separated by filtration and recrystallized from dimethylformamide to give 8,9-difluoro-2-methyl-7-amino-6-oxo-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (2.7 g) as yellow cubic crystals. m.p. 270°-274° C. (decomp.)

Quelle