HRID2211197

反应详情

EQUATION

反应方程式

HRID 2211197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Next, 4,4-bis[(trifluoromethyl)sulfonyl]-1-butene was prepared by adding 3 ml of allyl bromide to 31.3 millimoles of the bis[(trifluoromethyl)sulfonyl] methane potassium magnesium chloride in 35 ml of THF. The mixture was stirred at 70° C. under reflux for 8 hours. After removal of solvent by distillation under reduced pressure, 50 ml of 3N hydrochloric acid was added to the residue and the aqueous solution was extracted with ethyl ether. The ethyl ether solution was dried with anhydrous MgSO4. The ethyl ether was removed from the solution and the product was distilled at 0.02 torr.

WORKUP

后处理

  1. temperatureunder reflux for 8 hours
  2. customAfter removal of solvent
  3. distillationby distillation under reduced pressure, 50 ml of 3N hydrochloric acid
  4. additionwas added to the residue
  5. extractionthe aqueous solution was extracted with ethyl ether
  6. dry with materialThe ethyl ether solution was dried with anhydrous MgSO4
  7. customThe ethyl ether was removed from the solution
  8. distillationthe product was distilled at 0.02 torr