反应详情

A mixture of 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.5 g), β-picoline (11 ml) and 3-aminomethyl-4-methylpyrrolidine (0.5 g) was refluxed for 8.5 hours, then the reacting mixture was cooled to room temperature. To the mixture was added concentrated aqueous ammonia (100 ml) and concentrated under reduced pressure. To the residue was added dichloromethane-ether (1:3, 37 ml), the resulting precipitate was collected by filtration, washed with ethanol-ether (1:3), recrystallized from ethanol and further recrystallized from chloroform-methanol-concentrated aqueous ammonia (10:10:1) to give the title compound (0.14 g) as pale yellow powder, mp 245°-248° C.

1. temperaturewas refluxed for 8.5 hours
2. concentrationconcentrated under reduced pressure
3. additionTo the residue was added dichloromethane-ether (1:3, 37 ml)
4. filtrationthe resulting precipitate was collected by filtration
5. washwashed with ethanol-ether (1:3)
6. customrecrystallized from ethanol
7. customfurther recrystallized from chloroform-methanol-concentrated aqueous ammonia (10:10:1)