Ammonia → HCID 13960223, compound

Participants

Reaction Steps

4.01 g (0.01 mole) of 9-fluoro-5-methyl-8-(3-methyl-1-piperazinyl)-6,7-dihydro-1, 7-dioxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid ethyl ester was suspended in a mixture of 20 ml of ethanol and 20 ml of 6N hydrochloric acid, and this suspension was stirred at 80°-90° C. for 5 hours to hydrolyze the starting material. The resulting reaction solution was adjusted to pH 7-8 by the addition of 28% aqueous ammonia under cooling with ice. The precipitate which separated out was collected by filtration and recrystallized from a water-ethanol mixture (with a volume ratio of 1:1) to obtain 2.69 g (72.0% yield) of 9-fluoro-5-methyl-8-(3-methyl-1-piperazinyl)-6,7-dihydro-1, 7-dioxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid in the form of yellow crystals. These crystals had a melting point of 231°-234° C. (dec.) .

Provenance & Evidence