HRID274164

反应详情

EQUATION

反应方程式

HRID 274164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

100 g (0.455 mol) of 4-iodophenol and 54.6 g (1.365 mol) of sodium hydroxide are added to a mixture of 300 ml of THF and 30 ml of water. After stirring for about 1/2 hour, the mixture is evaporated in a rotary evaporator; this is repeated after the addition of 200 ml of toluene. The residue is taken up in 400 ml of THF. The mixture is cooled to 0° C., 47.1 g (0.545 mol) of chlorodifluoromethane are introduced, and the mixture is then stirred for 1 hour. It is then stirred at about +5° C. for 18 hours. The solution above the resulting slurry-like precipitate was decanted off. It was evaporated in a rotary evaporator, and the residue was chromatographed through a silica gel column, using petroleum ether as eluent.

WORKUP

后处理

  1. customthe mixture is evaporated in a rotary evaporator
  2. additionafter the addition of 200 ml of toluene
  3. stirringthe mixture is then stirred for 1 hour
  4. stirringIt is then stirred at about +5° C. for 18 hours
  5. customThe solution above the resulting slurry-like precipitate was decanted off
  6. customIt was evaporated in a rotary evaporator
  7. customthe residue was chromatographed through a silica gel column