反应详情

温度

42.5 °C

34.7 g of anhydrous K2CO3 (0.35 mol) was added to a solution of 64.2 g of ethyl 2-(3-cyano-2,4-dichloro-5-fluorobenzoyl)-3-cyclopropylaminoacrylate (0.173 mol) in 220 ml of DMF. The reacting mixture was stirred at 40-45° C. for 2.5 hours, and the reaction was monitored by TLC. The reactant was then poured into 800 ml of ice-water, filtered, washed with water (100 ml×2), and dried. The resultant solid was dissolved in 120 ml of 95% ethanol and then refluxed for 15 minutes, cooled, filtered and dried to afford 53.2 g of ethyl 8-cyano-1-cyclopropyl-7-chloro-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate (0.159 mol) as a white solid, mp 196-199° C., in 90.1% yield.

1. filtrationfiltered
2. washwashed with water (100 ml×2)
3. customdried
4. dissolutionThe resultant solid was dissolved in 120 ml of 95% ethanol
5. temperaturerefluxed for 15 minutes
6. temperaturecooled
7. filtrationfiltered
8. customdried