反应详情

温度

100 °C

To a solution of 2-(6-bromo-3-methoxypyridin-2-yl)-4-fluoro-1H-benzo[d]imidazole (350 mg, 1.12 mmol) in DMF (10 mL) was added LiCl (650 mg, 15.5 mmol) under N2 protection. The mixture was stirred on a pre-heated oil-bath at 100° C. overnight. After extracted with EtOAc, the organic phase was dried over Na2SO4 and concentrated. The residue was purified by prep-TLC (PE:EA=5:1) to give the product of 6-bromo-2-(4-fluoro-1H-benzo[d]imidazol-2-yl)pyridin-3-ol (200 mg, yield: 60%). 1H-NMR (DMSO-d6, 400 MHz) δ 13.75 (s, 1H), 12.70 (s, 1H), 7.64 (d, J=8.4 Hz, 1H), 7.50 (d, J=8.4 Hz, 1H), 7.41 (s, 1H), 7.30 (s, 1H), 7.12 (s, 1H). MS (M+H)+: 308/310.

1. extractionAfter extracted with EtOAc
2. dry with materialthe organic phase was dried over Na2SO4
3. concentrationconcentrated
4. customThe residue was purified by prep-TLC (PE:EA=5:1)