反应详情

The solution of 3.0 g of ethyl 3-cyclopropylamino-2-(2,6-dichloro-5-fluoropyridine-3-carbonyl)acrylate in 36.4 ml of anhydrous tetrahydrofuran was cooled to 10° C. 0.36 g (1.05 eq.) of 60% sodium hydride was added to the reaction mixture, which was then stirred for 18 hours at room temperature. The reaction mixture was cooled to 5˜10° C. 36.4 ml of water was added to the reaction mixture, which was then stirred for 30 minutes. The organic layer was filtered under a reduced pressure and washed with water. The resulting wet cake was dried under a reduced pressure at 50° C. for 5 hours to give 2.34 g of ethyl 7-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (Yield: 87.3%).

1. temperatureThe reaction mixture was cooled to 5˜10° C
2. stirringwas then stirred for 30 minutes
3. filtrationThe organic layer was filtered under a reduced pressure
4. washwashed with water
5. customThe resulting wet cake was dried under a reduced pressure at 50° C. for 5 hours