反应详情

温度

120 °C

6-(4-Methoxyphenyl)-5H-thieno[3,2-c]pyridin-4-one (9.1 g) was added to phosphorus oxychloride (90 g), and the mixture was heated at 120° C. for 3 hr. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate and water. The organic layer was washed with water, an aqueous solution of saturated sodium bicarbonate and brine, and dried over magnesium sulfate. The solvent was evaporate, and the resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system), to give the title compound as a white powder (6.6 g, yield; 73%).

1. customThe reaction solution was evaporated
2. additionto the resulting residue were added ethyl acetate and water
3. washThe organic layer was washed with water
4. dry with materialan aqueous solution of saturated sodium bicarbonate and brine, and dried over magnesium sulfate
5. customThe solvent was evaporate
6. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system)