反应详情

温度

110 °C

To the intermediate 6-methoxy-1,5-naphthyridin-4(1H)-one (15.0 g, 0.085 mol) was added POCl3 (300 mL) dropwise under nitrogen atmosphere at RT. The reaction mixture was heated to 110° C. with constant stirring. After 12 h, the mixture was concentrated in vacuo and azeotroped with toluene (2×100 mL). The residue was dissolved in ice-water (100 mL) and adjusted pH of the solution to 7 using 10% NaHCO3 solution, and extracted with EtOAc (4×100 mL). The combined organic extracts were washed with water (2×100 mL), saturated NaCl solution (100 mL), dried (Na2SO4), filtered and concentrated in vacuo.

1. concentrationthe mixture was concentrated in vacuo
2. customazeotroped with toluene (2×100 mL)
3. dissolutionThe residue was dissolved in ice-water (100 mL)
4. extractionextracted with EtOAc (4×100 mL)
5. washThe combined organic extracts were washed with water (2×100 mL), saturated NaCl solution (100 mL)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo