Reaktion #500240

Reaktionsgleichung

ethyl 9-[3-(3,4-dimethylphenyl)piperazin-1-yl]-8-fluoro-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylate

→

9-[3-(3,4-dimethylphenyl)piperazin-1-yl]-8-fluoro-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylic acid

Ausbeute 70.7%

Lösungsmittel

ethanol

potassium hydroxide

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction mixture was filtered
2. 2
   Sonstigeevaporated to dryness
3. 3
   workup.ADDITIONwas added
4. 4
   Temperaturthe medium was heated to 100° C.
5. 5
   Filtrationfiltered at high temperature
6. 6
   WaschenThe residue was washed 3 times with 25 cm3 of water

Vorschrift

A stirred suspension of 1.47 g of ethyl 9-[3-(3,4-dimethylphenyl)piperazin-1-yl]-8-fluoro-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylate in 25 cm3 of ethanol, 3.60 cm3 of 1 N aqueous potassium hydroxide and 15 cm3 of water was heated in the region of 100° C. for 4 hours. The reaction mixture was filtered, evaporated to dryness, the residue was suspended in 100 cm3 of water, the medium was acidified with 3.5 cm3 of a 1 N aqueous hydrochloric acid solution, 10 cm3 of ethanol was added, the medium was heated to 100° C. and filtered at high temperature. The residue was washed 3 times with 25 cm3 of water and then with 10 cm3 of ethanol. 0.98 g of 9-[3-(3,4-dimethylphenyl)piperazin-1-yl]-8-fluoro-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylic acid was obtained in the form of a yellow solid, which melted at 325° C.

Quelle