反应详情

7.0 g of ethyl 3-cyclopropylamino-2-(2,6-dichloro-5-fluoropyridine-3-carbonyl)acrylate was dissolved in 35 ml of acetonitrile under heating to 75˜80° C. 8.56 g (2.0 eq.) of K3PO4 was added in portions to the reaction mixture, which was then stirred at the same temperature for 1.5 hours. The reaction mixture was filtered under a reduced pressure and washed with 77 ml of dichloromethane. The filtrate was concentrated under a reduced pressure. The resulting residue was dissolved in 77 ml of dichloromethane and then washed with water. The organic layer was concentrated under a reduced pressure to give 6.17 g of ethyl 7-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (Yield: 98.5%).

1. temperatureunder heating to 75˜80° C
2. filtrationThe reaction mixture was filtered under a reduced pressure
3. washwashed with 77 ml of dichloromethane
4. concentrationThe filtrate was concentrated under a reduced pressure
5. dissolutionThe resulting residue was dissolved in 77 ml of dichloromethane
6. washwashed with water
7. concentrationThe organic layer was concentrated under a reduced pressure