HRID931536
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
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 stirred 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.
WORKUP
后处理
- temperatureThe brown solution was cooled to RT
- additionpoured onto ice
- filtrationThe resulting tan precipitate was collected by filtration
- washwashed sequentially with water (2 L), 1N NaOH (2.0 L) and ethanol (800 mL)
- stirringstirred vigorously for 1 hour
- filtrationThe mixture was filtered
- customdried under a vacuum