Potassium Phosphate, Tribasic → HCID 69374561, compound

Participants

Reaction Steps

45.69 g of (+) ethyl 2-(2,4-dichloro-3-nitro-5-fluorobenzoyl)-3-[(1-acetoxyprop-2(S)-yl)amino]acrylate was dissolved in 270 ml of acetonitrile under heating to 70˜75° C. 32.25 g (1.5 eq.) of K3PO4 was added in portions to the reaction mixture, which was then stirred at the same temperature for 12 hours. The reaction mixture was filtered under a reduced pressure and washed with 500 ml of dichloromethane. The filtrate was concentrated under a reduced pressure. The resulting residue was dissolved in 300 ml of dichloromethane and then washed with water. The organic layer was concentrated under a reduced pressure to give 46.6 g of (−) ethyl N-(acetoxy-prop-2(S)-yl)-6-fluoro-7-chloro-8-nitro-4-quinolone-3-carboxylate (Yield: 96.1%).

Provenance & Evidence