HRID662039
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
1-Bromo-3-methyl-2-(methyloxy)benzene (30.3 g, 0.15 mol), NBS (28.2 g, 0.16 mol), and BPO (1.83 g, 7.55 mmol) were suspended in 300 mL of CCl4, and the mixture was heated to 80° C. over night. After cooling to room temperature, the solution was filtrated and the solid was washed with CCl4 (30 mL×2). The filtrate was washed with NaHSO3 (aq. 250 mL×2), Na2CO3 (aq. 100 mL×2), brine (100 mL) and dried over Na2SO4. After removing the solvent, 41.4 g of the crude product was obtained (yield: 97.9%).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe solution was filtrated
- washthe solid was washed with CCl4 (30 mL×2)
- washThe filtrate was washed with NaHSO3 (aq. 250 mL×2), Na2CO3 (aq. 100 mL×2), brine (100 mL)
- dry with materialdried over Na2SO4
- customAfter removing the solvent