反应详情

温度

150 °C

A mixture of 4-benzyloxy-1H-pyridin-2-one (7.04 g, 35.0 mmols), 2-[(4-iodophenyl)oxy]tetrahydropyran (13.6 g, 44.8 mmols), cuprous iodide (2.1 g, 11.2 mmols), potassium carbonate (10.3 g, 73.5 mmols) and N,N-dimethylformamide (200 mL) was stirred overnight at 150° C. The reaction liquid was cooled to room temperature, into which water (1.2 L) was poured, and the formed insoluble matter was recovered by filtration. Chloroform (300 mL) was added to the insoluble matter, followed by another filtration. The filtered organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, ethyl acetate was added to the resulting residue. The precipitate was recovered by filtration and dried to provide the title compound (7.6 g, 58%).

1. customThe reaction liquid
2. additionwas poured
3. filtrationthe formed insoluble matter was recovered by filtration
4. additionChloroform (300 mL) was added to the insoluble matter
5. filtrationfollowed by another filtration
6. washThe filtered organic layer was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationConcentrating the solvent under reduced pressure, ethyl acetate
9. additionwas added to the resulting residue
10. filtrationThe precipitate was recovered by filtration
11. customdried