HRID2211197
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 8 hours
- customAfter removal of solvent
- distillationby distillation under reduced pressure, 50 ml of 3N hydrochloric acid
- additionwas added to the residue
- extractionthe aqueous solution was extracted with ethyl ether
- dry with materialThe ethyl ether solution was dried with anhydrous MgSO4
- customThe ethyl ether was removed from the solution
- distillationthe product was distilled at 0.02 torr