Cfc 113 → 2-(Difluoromethyl)-4,4,5-trifluoro-2-(trifluoromethyl)-1,3-dioxolane

HRID 328359노트

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HRID 328359 반응식
[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

참가 물질

5

실험 절차

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.

후처리

  1. additionwere added
  2. customAn 8° (Centigrade) exotherm was observed during the reaction
  3. filtrationThe mixture was filtered
  4. customleaving 59 g

출처 및 근거

ORD 기록
ord-a2c2e3f2cb6046a1a07c5467071a738f
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017519

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