HRID1963287

反应详情

EQUATION

反应方程式

HRID 1963287 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In a dried flask zinc powder (2.489 g, 38.07 mmol) was suspended in anhydrous tetrahydrofuran (50 mL) under nitrogen. The resulting suspension was warmed to 60° C., then 1,2-dibromoethane (0.126 mL, 1.46 mmol) was added and stirred at that temperature for 15 min. It was cooled to room temperature, then chlorotrimethylsilane (0.149 mL, 1.17 mmol) was added and stirred for 20 min. 1-(Bromomethyl)-2-(trifluoromethyl)benzene (4.46 mL, 29.28 mmol) in THF (2 mL) was added dropwise and stirring was continued at room temperature for 4 h. Stirring was switched off to let the precipitates settle. The supernatant was used in the next transformation.

WORKUP

后处理

  1. temperatureIt was cooled to room temperature
  2. stirringstirred for 20 min
  3. stirringstirring
  4. waitwas continued at room temperature for 4 h
  5. stirringStirring