反应详情

温度

60 °C

Sulfuric acid (1.6 L) was added to 2-(4-bromophenoxy)-5-methoxybenzoic acid (530 g, 1.6401 mol) at RT. The resulting dark mixture was heated to 60° C. for 1 hour. The brown solution was cooled to RT and poured onto ice while stirring. The resulting tan precipitate was collected by filtration, washed sequentially with water (2 L), 1N NaOH (2.0 L) and ethanol (800 mL). The derived solid was suspended in 2 L of acetone and stiffed vigorously for 1 hour. The mixture was filtered and dried under a vacuum to afford 1.3 kg of 2-bromo-7-methoxy-9H-xanthen-9-one as a white solid.

1. temperatureThe brown solution was cooled to RT
2. additionpoured onto ice
3. filtrationThe resulting tan precipitate was collected by filtration
4. washwashed sequentially with water (2 L), 1N NaOH (2.0 L) and ethanol (800 mL)
5. filtrationThe mixture was filtered
6. customdried under a vacuum