反应详情

The stirred mixture of 48.5 g of 2-amino-3-cyano-4-hydroxy-6-nitroquinoline and 550 mL of phosphoryl chloride was refluxed for 4 hours. The reaction mixture was concentrated to half of its volume and the residue was poured onto 1500 g of ice. The yellow precipitate was filtered off, washed with water to give 60.5 g of solid. 25 g of this solid was stirred at room temperature in 500 mL of 0.5 N HCl for 6 hours, then the precipitate was filtered off, washed with water to give 18.5 g of product, m.p.: >360° C. LC-MS: MH+ 249; Ret. time: 5.94 min.

1. temperaturewas refluxed for 4 hours
2. concentrationThe reaction mixture was concentrated to half of its volume
3. additionthe residue was poured onto 1500 g of ice
4. filtrationThe yellow precipitate was filtered off
5. washwashed with water