反応 #1755447

反応方程式

potassium hydroxide

2,2,3,4,4,4-hexafluorobutan-1-ol

1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride

→

2,2,3,4,4,4-hexafluorobutyl 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonate

溶媒

water

反応条件

後処理

1. 1
   その他The flask was equipped with a magnetic stirrer, cold water condenser
2. 2
   workup.ADDITIONthermocouple and a 250-mL addition funnel
3. 3
   その他did not exceed 35° C
4. 4
   workup.ADDITIONOnce the addition of the base
5. 5
   ろ過The precipitated salts were then filtered from the mixture
6. 6
   その他the lower liquid fluorochemical product phase was separated from the upper aqueous phase
7. 7
   その他were removed by atmospheric distillation

実験手順

2,2,3,4,4,4-hexafluorobutan-1-ol (202 g, 1.1 mol, obtained from Sinochem Corp., Beijing, China), 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride (332 g, 1.1 mol, obtained from 3M Company of Saint Paul, Minn.) and water (300 g) were combined in a 3-L, 3-necked round bottom flask. The flask was equipped with a magnetic stirrer, cold water condenser, thermocouple and a 250-mL addition funnel. Aqueous potassium hydroxide (149.3 g, 45 weight percent, 1.22 equivalents) was added dropwise via an addition funnel at such a rate that the temperature did not exceed 35° C. Once the addition of the base was complete the mixture was stirred for 16 hours at room temperature. The precipitated salts were then filtered from the mixture and the lower liquid fluorochemical product phase was separated from the upper aqueous phase. Unreacted 2,2,3,4,4,4-hexafluorobutan-1-ol and 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride were removed by atmospheric distillation.

出典