反应详情

温度

40 °C

To a stirred solution of 4-[5-fluoro-3-[4-(2-methylimidazol-1-yl)benzyloxy]-phenyl]-3,4,5,6-tetrahydro-2H-pyran-4-carboxamide (Example 5) in THF (10 ml) was added phosphorus pentasulfide (236 mg, 0.53 mmol) and sodium bicarbonate (176 mg, 2.1 mmol). The resulting mixture was heated at 40° C. for 4 hr. The mixture was concentrated in vacuo. To the residue was added water (100 ml) and the mixture was extracted with dichloromethane (2×100 ml). The combined organic extracts were dried over sodium sulfate and concentrated in vacuo. The residue was purified on column chromatography (LiChropprep --NH2) and then by p-TLC eluting with dichloromethane-methanol (10:1) to afford 38 mg of the titled compound as white solids.

1. concentrationThe mixture was concentrated in vacuo
2. additionTo the residue was added water (100 ml)
3. extractionthe mixture was extracted with dichloromethane (2×100 ml)
4. dry with materialThe combined organic extracts were dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified on column chromatography (LiChropprep --NH2)
7. washby p-TLC eluting with dichloromethane-methanol (10:1)