反応 #985271

反応方程式

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

溶媒

dioxane

dioxane

反応条件

後処理

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
   その他a complete reaction (usually an hour)
5. 5
   抽出The crude product was extracted into diethyl ether (3×50 cm3)
6. 6
   乾燥dried (MgSO4)
7. 7
   その他The solvent was removed in vacuo
8. 8
   その他the pure product was obtained by reduced pressure distillation as a colourless liquid

実験手順

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.

出典