HRID749995

反应详情

EQUATION

反应方程式

HRID 749995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 4-(4-methoxy-phenoxy)-biphenyl (3.2 g, 11.6 mmol) in anhydrous dichloromethane (60 mL) at −78° C. was added borontribromide (1M solution in dichloromethane) (7.52 g, 30 mmol) over a period of 15 min. The reaction mixture was stirred at −78° C. for 1 h, warmed to rt and stirred at rt for 1 h. The mixture was cooled to 0-5° C. Cold water (125 mL) was added over a period of 10 min and the mixture was extracted with dichloromethane (250 mL). The organic layer was dried over anhydrous Na2SO4. The crude mixture was purified by silica gel flash chromatography to obtain the title product (375 mg, 12%).

WORKUP

后处理

  1. temperaturewarmed to rt
  2. stirringstirred at rt for 1 h
  3. temperatureThe mixture was cooled to 0-5° C
  4. extractionthe mixture was extracted with dichloromethane (250 mL)
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. customThe crude mixture was purified by silica gel flash chromatography