反应详情

温度

85 °C

To 2.2 g of 1-(1,3-dioxolan-2-ylmethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one, 20 mL of an 80% aqueous trifluoroacetic acid solution was added, and the mixture was stirred at 80 to 90° C. for 3 hours. Thereto was added 10 mL of an 80% aqueous trifluoroacetic acid solution, and the mixture was stirred at 80 to 90° C. for 2 hours, then, 10 mL of an 80% aqueous trifluoroacetic acid solution was further added, and the mixture was stirred at the same temperature for 9 hours. The reaction mixture was cooled to room temperature, and the solvent was then distilled off under reduced pressure. To the resultant residue, a 2 mol/L aqueous sodium hydroxide solution was added and adjusted to pH 8.0, and chloroform and methanol were added thereto. The organic layer was separated, and the aqueous layer was extracted with a mixed solution of chloroform and methanol twice. The organic layer and the extract were combined, the resultant solution was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Diethyl ether and hexane were added to the resultant residue, and the solid was filtered off to obtain 1.5 g of 7-fluoro-1-(2-hydroxy-2-methoxyethyl)-1,5-naphthyridin-2(1H)-one as a light brown solid.

1. stirringthe mixture was stirred at 80 to 90° C. for 2 hours
2. stirringthe mixture was stirred at the same temperature for 9 hours
3. temperatureThe reaction mixture was cooled to room temperature
4. distillationthe solvent was then distilled off under reduced pressure
5. additionTo the resultant residue, a 2 mol/L aqueous sodium hydroxide solution was added
6. additionwere added
7. customThe organic layer was separated
8. extractionthe aqueous layer was extracted with a mixed solution of chloroform and methanol twice
9. dry with materialthe resultant solution was dried over anhydrous magnesium sulfate
10. distillationthe solvent was distilled off under reduced pressure
11. additionDiethyl ether and hexane were added to the resultant residue
12. filtrationthe solid was filtered off