HRID256088

反应详情

EQUATION

反应方程式

HRID 256088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To an ethanol solution of sodium ethylate obtained by dissolving 0.7 g of metallic sodium in 50 ml of ethanol were added 8.9 g of 2,6-dichloro-4-(2,2,2,-trifluoroethylthio)-phenol and 20 g of ethylene bromide. The mixture was stirred at 40° C. for 2 hours and under reflux for 4 hours. Ethanol and the excess of ethylene bromide were evaporated. The residue was taken into 150 ml of toluene, washed with a 5% aqueous solution of potassium hydroxide and water in this sequence, and dried over anhydrous sodium sulfate. Toluene was evaporated, and the residue was distilled under reduced pressure to give 7.2 g of 2-[2,6-dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl bromide with the b.p.=124°-126° C./0.8 mmHg.

WORKUP

后处理

  1. temperatureunder reflux for 4 hours
  2. customEthanol and the excess of ethylene bromide were evaporated
  3. washwashed with a 5% aqueous solution of potassium hydroxide and water in this sequence
  4. dry with materialdried over anhydrous sodium sulfate
  5. customToluene was evaporated
  6. distillationthe residue was distilled under reduced pressure