反応 #1596976

反応方程式

potassium carbonate

ethylene chlorohydrin

hexafluoroacetone

t-butyl methyl ether

→

2,2-bis(trifluoromethyl)-1,3-dioxolane

収率 62.7%

溶媒

water

反応条件

後処理

1. 1
   その他Into a 300 mL three-necked flask equipped with a gas-inlet tube, a reflux condenser
2. 2
   温度by cooling with ice
3. 3
   workup.ADDITIONAfter completion of the addition
4. 4
   workup.ADDITIONafter completion of the addition
5. 5
   workup.STIRRINGthe whole was stirred as it
6. 6
   その他an organic layer was separated by two-layer separation in a separating funnel
7. 7
   workup.DISTILLATIONThe resulting organic layer was subjected to distillation under normal pressure
8. 8
   その他to collect a fraction of 106° C. to 107° C.

実験手順

Into a 300 mL three-necked flask equipped with a gas-inlet tube, a reflux condenser, and a thermometer was charged 10.0 g (0.12 mol) of ethylene chlorohydrin beforehand, followed by cooling with ice. Then, 20.0 g (0.12 mol) of hexafluoroacetone was added through the gas-inlet tube. After completion of the addition, the whole was stirred for 15 minutes as it was and then 100 mL of t-butyl methyl ether was added. Then, 16.6 g (0.12 mol) of potassium carbonate was added portionwise over a period of 1 hour and, after completion of the addition, the whole was stirred as it was. The resulting mixture was poured into 100 mL of water and an organic layer was separated by two-layer separation in a separating funnel. The resulting organic layer was subjected to distillation under normal pressure to collect a fraction of 106° C. to 107° C. to obtain 15.8 g (purity 99%, yield 62.0%) of 2,2-bis(trifluoromethyl)-1,3-dioxolane (fluorinated acetal (E)).

出典