Reaktion #521877

Reaktionsgleichung

9-chloro-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid

2-oxo-piperazine

→

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

Ausbeute 32.6%

Lösungsmittel

hexamethylphosphoric triamide

hexamethylphosphoric triamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas reacted at 140°-150° C. on an oil bath for 6 hours
2. 2
   workup.DISTILLATIONwas distilled off and to the residue
3. 3
   workup.ADDITIONwas added ethyl acetate
4. 4
   Sonstigeto form crystals, which
5. 5
   Filtrationthen were collected by filtration
6. 6
   SonstigeThe crystals thus obtained
7. 7
   Sonstigewere recrystallized twice each from dimethylformamide

Vorschrift

A mixture of 6 g of 9-chloro-8-fluoro-2-methyl-1,2-dihydro-6-oxo-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid, 8.6 g of 2-oxo-piperazine and 60 ml of hexamethylphosphoric triamide was reacted at 140°-150° C. on an oil bath for 6 hours. After completion of reaction, hexamethylphosphoric triamide was distilled off and to the residue was added ethyl acetate to form crystals, which then were collected by filtration. The crystals thus obtained were recrystallized twice each from dimethylformamide to give 2.4 g of 9-(3-oxo-1-piperazinyl)-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., white rhombic crystals.

Quelle