反应详情

温度

110 °C

7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (168 mg, 0.511 mmol) is dissolved in 2,2-difluoropropionic acid (562 mg), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 110° C. for 4 h. The reaction mixture is cooled to room temperature, diluted with water (10 ml) and extracted with ethyl acetate (3×30 ml). The ethyl acetate extracts are combined and washed with saturated sodium bicarbonate solution (2×40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), treated with decolourising charcoal (50 mg), filtered and evaporated to give a colourless solid. This is sonicated with n-hexane/diethyl ether and filtered to give a cream-coloured powder.

1. temperatureThe reaction mixture is cooled to room temperature
2. extractionextracted with ethyl acetate (3×30 ml)
3. washwashed with saturated sodium bicarbonate solution (2×40 ml) and saturated brine (40 ml)
4. dry with materialThe organic layer is dried (MgSO4)
5. additiontreated with decolourising charcoal (50 mg)
6. filtrationfiltered
7. customevaporated
8. customto give a colourless solid
9. filtrationfiltered
10. customto give a cream-coloured powder