反应详情

温度

80 °C

The 4-acetyl-2-chloro-5-hydroxybenzonitrile (4.9 g, 25 mmol) was dissolved in acetic acid (61.2 mL), and the N-iodosuccinimide (6.8 g, 30 mmol) was added. The reaction was heated to 80° C. and, after heating for 18 hrs, the reaction was concentrated in vacuo to remove the acetic acid. The residue was taken up in ethyl acetate, washed with sodium bicarbonate water, brine, dried over magnesium sulfate and concentrated to give a dark oil. The crude product was purified by FCC on silica gel eluting hexane:ethyl acetate gradient to give 4-acetyl-6-chloro-3-hydroxy-2-iodobenzonitrile as a yellow solid (5.3 g, 66%).

1. temperatureafter heating for 18 hrs
2. concentrationthe reaction was concentrated in vacuo
3. customto remove the acetic acid
4. washwashed with sodium bicarbonate water, brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customto give a dark oil
8. customThe crude product was purified by FCC on silica gel
9. washeluting hexane