HRID491412

反应详情

EQUATION

反应方程式

HRID 491412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Bromo-4-methyl anisole 14 (2.2 mL, 14.9 mmol) was dissolved in dichlomethane (30 mL) and N-bromosuccinimide (3.75 g, 16.4 mmol) was added followed by AIBN (26.0 mg). The reaction was heated to reflux for 19 hrs., then cooled to room temperature and the precipitate was filtered off. The filtrate was diluted with dichloromethane and washed with 0.5 M aqueous sodium bicarbonate, followed by water. The organic mixture was dried over sodium sulfate, filtered and concentrated under vacuum to yield 15 (4.16 g, 100%). The benzyl bromide was used as the crude material without further purification.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 19 hrs
  4. filtrationthe precipitate was filtered off
  5. additionThe filtrate was diluted with dichloromethane
  6. washwashed with 0.5 M aqueous sodium bicarbonate
  7. dry with materialThe organic mixture was dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum