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Octane → 2,3-Difluoro-2-(pentafluoroethyl)-3-(trifluoromethyl)oxirane

HRID 1244875
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HRID 1244875 반응식
CCCCCCCC.[F:9][C:10]([F:24])([F:23])[C:11]([F:22])(Br)[C:12](=[O:20])[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15].[F:25]C(F)(F)C(=O)C(F)(Br)C(F)(F)C(F)(F)F>>[F:9][C:10]([F:24])([F:23])[C:11]1([F:22])[O:20][C:12]1([F:25])[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 356Octane2회HCID 219240182-Bromo-1,1,1,2,4,4,5,5,5-nonafluoropentan-3-oneHCID 21924019HCID 21924019, 화합물

생성물 1

HCID 125209252,3-Difluoro-2-(pentafluoroethyl)-3-(trifluoromethyl)oxirane

실험 절차

The distillate was subjected to flash chromatography on silica gel using octane as an eluant. The column effluent containing primarily octane and the mixture of perfluoro-2-bromo-3-pentanone and perfluoro-3-bromo-2-pentanone was then subjected to two vacuum distillations at a pressure of 56 and 100 torr, respectively, to separate the bromoperfluoroketones from the bulk of the octane. The low-boiling fractions from the vacuum distillations were then re-distilled at atmospheric pressure. The fractions collected at a head temperature of 71.2–72.8° C. were combined. The product was a mixture of perfluoro-2-bromo-3-pentanone and perfluoro-3-bromo-2-pentanone in molar ratio of 1.0 to 1.12 with overall purity of >98 GC area %.

후처리

  1. customrespectively, to separate the bromoperfluoroketones from the bulk of the octane
  2. distillationThe low-boiling fractions from the vacuum distillations were then re-distilled at atmospheric pressure
  3. customThe fractions collected at a head temperature of 71.2–72.8° C.
  4. additiona mixture of perfluoro-2-bromo-3-pentanone and perfluoro-3-bromo-2-pentanone in molar ratio of 1.0 to 1.12 with overall purity of >98 GC area %

출처 및 근거

ORD 기록
ord-802deb83f5ff4ba59d3e1b4b973826ff
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122704B2

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