反应详情

温度

120 °C

A mixture of 136 mg of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 180 mg of 4-aminoisoindoline, and 1.5 ml of anhydrous DMF was heated at 120° C. for 1.5 hours while stirring. The resulting reaction mixture was evaporated under reduced pressure to dryness. 20 ml of chloroform and 10 ml of 5% acetic acid was added to the residue, and the mixture was stirred. Deposited crystals were collected by filtration, washed with water and ethanol. The chloroform layer was separated, washed with brine, dried over anhydrous sodium sulfate, and condensed. The residue was crystallized by the addition of hot ethanol. After cooling the mixture, the crystals were collected by filtration. These crystals were combined with those collected above and were recrystallized from a mixed solvent of chloroform, methanol, and ethanol to obtain 123 mg of the target compound.

1. customThe resulting reaction mixture
2. customwas evaporated under reduced pressure to dryness
3. addition20 ml of chloroform and 10 ml of 5% acetic acid was added to the residue
4. stirringthe mixture was stirred
5. filtrationDeposited crystals were collected by filtration
6. washwashed with water and ethanol
7. customThe chloroform layer was separated
8. washwashed with brine
9. dry with materialdried over anhydrous sodium sulfate, and condensed
10. customThe residue was crystallized by the addition of hot ethanol
11. temperatureAfter cooling the mixture
12. filtrationthe crystals were collected by filtration
13. customthose collected above and
14. customwere recrystallized from a mixed solvent of chloroform, methanol, and ethanol