HRID1768878

反应详情

EQUATION

反应方程式

HRID 1768878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-80 °C

PROCEDURE

实验过程

In 1 l four-necked flask having a gas supplying tube, 200 ml of n-hexane, 75 ml of dry diethyl ether and 24.6 g (0.1 mol) of 4-(n-propyl)iodobenzene were introduced under a nitrogen atmosphere, and then 86.2 ml of a hexane solution of n-butyl lithium (1.16 mol) was dropwise added thereto under stirring at -80° C. Then, while the reaction system was maintained at -80° C., 10 g (0.1 mol) of tetrafluoroethylene was introduced under vigorously stirring in 30 minutes. The reaction solution was stirred further for one hour and poured into ice water and neutralized with dilute hydrochloric acid, and then the organic layer was separated. The aqueous layer was extracted with methylene chloride, and the extract was combined to the organic layer, followed by drying. The solvent was distilled off to obtain 12 g (yield: 60%) of 1-(4-n-propylphenyl)-1,2,2-trifluoroethylene.

WORKUP

后处理

  1. customIn 1 l four-necked flask having
  2. temperatureThen, while the reaction system was maintained at -80° C.
  3. stirringunder vigorously stirring in 30 minutes
  4. stirringThe reaction solution was stirred further for one hour
  5. customthe organic layer was separated
  6. extractionThe aqueous layer was extracted with methylene chloride
  7. customby drying
  8. distillationThe solvent was distilled off