تفاعل #985271

معادلة التفاعل

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

المذيبات

dioxane

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةduring reflux
2. 2
   workup.ADDITIONAfter addition
3. 3
   درجة الحرارةthe reaction mixture was refluxed for a period of time until the GLC analysis
4. 4
   أخرىa complete reaction (usually an hour)
5. 5
   استخلاصThe crude product was extracted into diethyl ether (3×50 cm3)
6. 6
   تجفيفdried (MgSO4)
7. 7
   أخرىThe solvent was removed in vacuo
8. 8
   أخرىthe pure product was obtained by reduced pressure distillation as a colourless liquid

الإجراء التجريبي

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.

المصدر