反应详情

温度

25 °C

To a stirred solution of 2,6-dibromo-4-fluorophenol (214.5 g, 0.794 mol) in acetone (4.3 L), potassium carbonate (120.6 g, 0.874 mol) and methyl iodide (54.4 mL, 0.874 mol) were added at room temperature. The mixture was heated to reflux for 1.5 hours cooled to 25° C. and filtered, washing the filter cake with dichloromethane (2×1.5 L). The filtrate was concentrated in vacuo at 40° C. The crude product was slurred in dichloromethane (1 L) for 30 minutes at 25° C., filtered and concentrated in vacuo at 40° C. to give 1,3-Dibromo-5-fluoro-2-methoxybenzene as an off-white crystalline solid (223.3 g, 98.9%).

1. temperatureThe mixture was heated
2. temperatureto reflux for 1.5 hours
3. filtrationfiltered
4. washwashing the filter cake with dichloromethane (2×1.5 L)
5. concentrationThe filtrate was concentrated in vacuo at 40° C
6. filtrationfiltered
7. concentrationconcentrated in vacuo at 40° C.