反应详情

温度

75 °C

A mixture of 7-bromo-3-chloro-5H-chromeno[2,3-c]pyridin-5-one (20 g, 64.4 mmol), 2-methyl-2-propanesulfinamide (23.42 g, 193 mmol) and titanium (IV) ethoxide (45.3 mL, 219 mmol) in dry THF 250 mL was heated at 75° C. overnight. The mixture was cooled to RT, then brine was added while stirring. The resulting suspension was filtered through celite, and the solid was washed with EtOAc. The filtrate was washed with brine, dried over sodium sulfate and concentrated. The crude material was purified by column chromatography with gradient of 0-30% EtOAc/Hexane to give the desired product as an orange solid. MS m/z=415.0 [M+H]+.

1. temperatureThe mixture was cooled to RT
2. filtrationThe resulting suspension was filtered through celite
3. washthe solid was washed with EtOAc
4. washThe filtrate was washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe crude material was purified by column chromatography with gradient of 0-30% EtOAc/Hexane