反応 #415541

反応方程式

2-Difluoromethyl-2-trifluoromethyl-1,3-dioxolane

K2CO3

fluorine

fluorine

1,2,2-trifluoroperchloroethane

fluorine

→

2-difluoromethyl-2-trifluoromethyl-4,4,5-trifluoro-1,3-dioxolane

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   その他An 8° (Centigrade) exotherm was observed during the reaction
3. 3
   ろ過The mixture was filtered
4. 4
   その他leaving 59 g

実験手順

2-Difluoromethyl-2-trifluoromethyl-1,3-dioxolane (50 g.) was placed in a 500 ml. flask along with 1,2,2-trifluoroperchloroethane (Freon 113) (425 ml.) and the solution cooled to -20° C. The mixture was fluorinated with 20% fluorine in argon at a fluorine rate of 0.1 mole per hour until about 1.5 moles of fluorine were added. An 8° (Centigrade) exotherm was observed during the reaction. The acidic mixture was stirred over K2CO3 until the vapors above the mixture no longer tested strongly acidic. The mixture was filtered and Freon 113 was stripped out of the filtrate, leaving 59 g. of crude product. By preparative chromatography pure 2-difluoromethyl-2-trifluoromethyl-4,4,5-trifluoro-1,3-dioxolane (12 g.) was isolated from the crude material.

出典