反应详情

To a solution of 3-(4-chlorophenyl)-8-fluoro-7-(2-hydroxyethylamino)-2-isopropyl-chromen-4-one (0.195 g, 0.52 mmol) in dimethylformamide (5 ml) is added sodium hydride (0.053 g, 1.32 mmol, 60% dispersion in mineral oil, 2.55 eq.). The mixture is irradiated in a microwave instrument at 150° C. for 70 min. The solvent is removed by evaporation in vacuo to afford a brown oil. This is dissolved in hot ethyl acetate and allowed to cool to room temperature, whereupon a brown solid precipitates. More product can be recovered from the mother liquor by flash chromatography (cyclohexane/ethyl acetate=9:1). The solid products are combined and dried at 60° C. overnight under high vacuum to afford the title compound.

1. customThe mixture is irradiated in a microwave instrument at 150° C. for 70 min
2. customThe solvent is removed by evaporation in vacuo
3. customto afford a brown oil
4. customprecipitates
5. customMore product can be recovered from the mother liquor by flash chromatography (cyclohexane/ethyl acetate=9:1)
6. customdried at 60° C. overnight under high vacuum