반응 #1440284

반응 방정식

(+) ethyl 2-(2,4-dichloro-3-nitro-5-fluorobenzoyl)-3-[(1-acetoxyprop-2(S)-yl)amino]acrylate

K3PO4

→

ethyl N-(acetoxy-prop-2(S)-yl)-6-fluoro-7-chloro-8-nitro-4-quinolone-3-carboxylate

수율 95.7%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도under heating to 75˜80° C
2. 2
   여과The reaction mixture was filtered under a reduced pressure
3. 3
   세척washed with 60 ml of dichloromethane
4. 4
   농축The filtrate was concentrated under a reduced pressure
5. 5
   workup.DISSOLUTIONThe resulting residue was dissolved in 50 ml of dichloromethane
6. 6
   세척washed with water
7. 7
   농축The organic layer was concentrated under a reduced pressure

실험 절차

3.0 g of (+) ethyl 2-(2,4-dichloro-3-nitro-5-fluorobenzoyl)-3-[(1-acetoxyprop-2(S)-yl)amino]acrylate was dissolved in 15 ml of acetonitrile under heating to 75˜80° C. 2.12 g (1.5 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 60 ml of dichloromethane. The filtrate was concentrated under a reduced pressure. The resulting residue was dissolved in 50 ml of dichloromethane and then washed with water. The organic layer was concentrated under a reduced pressure to give 2.64 g of (−) ethyl N-(acetoxy-prop-2(S)-yl)-6-fluoro-7-chloro-8-nitro-4-quinolone-3-carboxylate (Yield: 95.7%)

출처