反应详情

In 1 ml of toluene was suspended 47 mg of ethyl 7-bromo-1-cyclopropyl-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate, and to this suspension were added 74 mg of 2-(p-toluenesulfonyl)-5-tributylstannylisoindoline and 1.5 mg of tetrakis(triphenylphosphine)palladium (0), after which the resulting mixture was heated under reflux for 18 hours under a nitrogen atmosphere. The reaction mixture was concentrated under reduced pressure, and the residue obtained was purified by a column chromatography (eluent: n-hexane:ethyl acetate=1:1), and diethyl ether was then added thereto, after which the crystals formed were collected by filtration, to obtain 27 mg of colorless, crystalline ethyl 1-cyclopropyl-6-fluoro-8-methyl-7-[2-(p-toluenesulfonyl)isoindolin-5-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylate.

1. temperatureafter which the resulting mixture was heated
2. temperatureunder reflux for 18 hours under a nitrogen atmosphere
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customthe residue obtained
5. customwas purified by a column chromatography (eluent: n-hexane:ethyl acetate=1:1), and diethyl ether
6. additionwas then added
7. customafter which the crystals formed
8. filtrationwere collected by filtration