反应详情

To a stirring solution of compound 1.10 (12 g, 83.3 mmol) in acetone (200 mL) was added AgNO3 (1.34 g, 7.9 mmol) and the the reaction was stirred for 30 min. NBS (17.7 g, 99.96 mmol) was then added and the reaction mixture was stirred at 20° C. for 14 hr. Solids were removed by filtration and the filtrate was concentrated under reduced pressure to give a crude, which was purified by flash chromatography (silica gel/ethyl acetate in petroleum ether 5%-10% v/v) to give compound 1.11 as a white solid (14 g, 76%). 1H NMR (400 MHz, DMSO-d6) δ 7.95 (d, J=8, 2H), 7.62 (d, J=8, 2H), 2.58 (s, 3H).

1. stirringthe reaction mixture was stirred at 20° C. for 14 hr
2. customSolids were removed by filtration
3. concentrationthe filtrate was concentrated under reduced pressure
4. customto give a crude, which
5. customwas purified by flash chromatography (silica gel/ethyl acetate in petroleum ether 5%-10% v/v)