HRID657337

反应详情

EQUATION

反应方程式

HRID 657337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling to room temperature
  2. filtrationthe solution was filtrated
  3. washthe solid was washed with CCl4 (30 mL×2)
  4. washThe filtrate was washed with NaHSO3 (aq. 250 mL×2), Na2CO3 (aq. 100 mL×2), brine (100 mL)
  5. dry with materialdried over Na2SO4
  6. customAfter removing the solvent