反应详情

A 3 g portion of 2-(5-bromo-2-thienyl)piperazine was suspended in 8 ml of dry pyridine. An 820 mg portion of 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid was added and the mixture was heated in a pressure bottle, under argon, at 120°-130° C. for 18 hours, then cooled, filtered and evaporated to dryness. The residue was evaporated from toluene and this residue purified by chromatography, eluting with chloroform:water saturated methanol (9:1). The appropriate fractions were combined, evaporated and recrystallized from dimethylformamide-ether, giving 440 mg of the desired product, mp 233°-235° C. (dec.).

1. temperaturethe mixture was heated in a pressure bottle, under argon, at 120°-130° C. for 18 hours
2. temperaturecooled
3. filtrationfiltered
4. customevaporated to dryness
5. customThe residue was evaporated from toluene
6. customthis residue purified by chromatography
7. washeluting with chloroform
8. customevaporated
9. customrecrystallized from dimethylformamide-ether