反应 #985271

反应方程式

AIBN

4iodo-6,6,7,7,8,8,9,9,9-nonafluorononan-1-ol

phosphorous acid

triethylamine

→

6,6,7,7,8,8,9,9,9-Nonafluorononan-1-ol

溶剂

dioxane

dioxane

反应条件

后处理

1. 1
   温度during reflux
2. 2
   workup.ADDITIONAfter addition
3. 3
   温度the reaction mixture was refluxed for a period of time until the GLC analysis
4. 4
   其他a complete reaction (usually an hour)
5. 5
   萃取The crude product was extracted into diethyl ether (3×50 cm3)
6. 6
   干燥dried (MgSO4)
7. 7
   其他The solvent was removed in vacuo
8. 8
   其他the pure product was obtained by reduced pressure distillation as a colourless liquid

实验过程

A solution of AIBN (4.9 g, 30 mmol) in dioxane (150 cm3) was added dropwise into a solution of 4iodo-6,6,7,7,8,8,9,9,9-nonafluorononan-1-ol (Preparation 1B, 25 g, 58 mmol), phosphorous acid (19.1 g, 0.29 mol) and triethylamine (32.3 g, 0.32 mol) in dioxane (150 cm3) under an atmosphere of nitrogen during reflux. After addition, the reaction mixture was refluxed for a period of time until the GLC analysis revealed a complete reaction (usually an hour). The crude product was extracted into diethyl ether (3×50 cm3) and dried (MgSO4). The solvent was removed in vacuo and the pure product was obtained by reduced pressure distillation as a colourless liquid.

来源