反应详情

A solution of 2-(4-bromo-2,6-difluorophenyl)acetonitrile (0.5 g, 2.155 mmol) in H2SO4 (3 mL, 56.3 mmol) and H2O (3 mL, 167 mmol) was stirred at 60° C. for 16 h. After LCMS analysis showed the starting material had disappeared, the mixture was dissolved in H2O (20 mL) and extracted by EA (2×30 mL). The organic layer was dried over Na2SO4, filtered and concentrated. The crude material was purified by silica column chromatography (PE/EA=3/1 to 1/1) to yield 2-(4-bromo-2,6-difluorophenyl)acetic acid (0.3 g, 0.718 mmol, 33.3% yield): 1H NMR (400 MHz, CD3OD) δ 7.13-7.05 (m, 2H), 3.71 (s, 2H).

1. extractionextracted by EA (2×30 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude material was purified by silica column chromatography (PE/EA=3/1 to 1/1)