Cfc 113 → 2-(Difluoromethyl)-4,4,5-trifluoro-2-(trifluoromethyl)-1,3-dioxolane
反応式
[F:1][CH:2]([F:12])[C:3]1([C:8]([F:11])([F:10])[F:9])[O:7]CC[O:4]1.FF.C([O-])([O-])=O.[K+].[K+].[F:21][C:22](Cl)(Cl)[C:23](Cl)([F:25])[F:24]>>[F:1][CH:2]([F:12])[C:3]1([C:8]([F:11])([F:10])[F:9])[O:7][C:23]([F:25])([F:24])[CH:22]([F:21])[O:4]1参加物
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.
後処理
- additionwere added
- customAn 8° (Centigrade) exotherm was observed during the reaction
- filtrationThe mixture was filtered
- customleaving 59 g
出典と根拠
- ORDレコード
- ord-a2c2e3f2cb6046a1a07c5467071a738f
- 出典データセット
- uspto-grants-1977_04
- 特許番号
- US04017519
反応ノート
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