反应详情

A mixture of 1-ethyl-6,7-dichloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid 2.86 g (0.01 mole), N-methylpiperazine 10 g (0.1 mole) and 15 ml water was heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours. After cooling, the reaction mixture was evaporated under vacuum and acidified with acetic acid. Insoluble matters were filtered off and the filtrate was neutralized with an aqueous solutiong of NaOH to pH 7, extracted with CHCl3, dried with anhydrous Na2SO4, and the solvent was distilled off. The residue was recrystallized from a mixed solvent of CHCl3 and benzene to give 1.05 g (30%) of 1-ethyl-6-chloro-7-(4-methyl-1-piperazinyl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid. Colorless needles.

1. temperaturewas heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours
2. temperatureAfter cooling
3. customthe reaction mixture was evaporated under vacuum
4. filtrationInsoluble matters were filtered off
5. extractionextracted with CHCl3
6. dry with materialdried with anhydrous Na2SO4
7. distillationthe solvent was distilled off
8. customThe residue was recrystallized from a mixed solvent of CHCl3 and benzene