反应详情

温度

80 °C

Acetic acid (20 ml) is added to polyphosphoric acid (˜25 g) heated to 80° C. The viscous solution is stirred vigorously for 5 min. 7-azido-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (1.0 g, 2.95 mmol) is added portionwise over a period of 10 min. The reaction mixture is heated at 120° C. for 3 h, cooled to room temperature and poured into water (200 ml), and the product is extracted with CH2Cl2. The organic phase is washed with water and brine, dried (MgSO4) and filtered. Methanol (30 ml) is added, followed by partial evaporation in vacuo to give a precipitate, which is isolated by filtration.

1. temperatureThe reaction mixture is heated at 120° C. for 3 h
2. temperaturecooled to room temperature
3. extractionthe product is extracted with CH2Cl2
4. washThe organic phase is washed with water and brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. additionMethanol (30 ml) is added
8. customfollowed by partial evaporation in vacuo
9. customto give a precipitate
10. customwhich is isolated by filtration