反应详情

温度

120 °C

7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (80 mg, 0.243 mmol) is dissolved in glacial acetic acid (1.5 ml), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 120° C. for 90 min. The reaction mixture is cooled to room temperature, diluted with ethyl acetate (50 ml) and washed with saturated sodium bicarbonate solution (3×40 ml), water (40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), filtered and evaporated to give a brown solid. This is triturated with ethyl acetate containing a few drops of methanol and filtered to give a pale yellow powder.

1. temperatureThe reaction mixture is cooled to room temperature
2. washwashed with saturated sodium bicarbonate solution (3×40 ml), water (40 ml) and saturated brine (40 ml)
3. dry with materialThe organic layer is dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto give a brown solid
7. customThis is triturated with ethyl acetate containing a few drops of methanol
8. filtrationfiltered
9. customto give a pale yellow powder