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Carbon tetrafluoride → Perfluoro 4,4-dimethyl-3-isopropyl-2-pentene

HRID 50411
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[F:1]C(F)(F)C(C(F)(F)F)=C(C(F)(F)C(F)(F)F)C(F)(C(F)(F)F)C(F)(F)F.FC([Si](C)(C)C)(F)F.[F-].[K+].FC(F)(F)F.[F:43][C:44]([F:75])([F:74])[C:45](C(F)(F)F)=[C:46]([C:60]([F:69])([C:65]([F:68])([F:67])[F:66])[C:61]([F:64])([F:63])[F:62])[C:47]([C:56]([F:59])([F:58])[F:57])([C:52]([F:55])([F:54])[F:53])[C:48]([F:51])([F:50])[F:49]>CN(C)C=O>[F:75][C:44]([F:43])([F:74])[C:45]([F:1])=[C:46]([C:60]([F:69])([C:61]([F:64])([F:62])[F:63])[C:65]([F:67])([F:68])[F:66])[C:47]([C:56]([F:59])([F:57])[F:58])([C:48]([F:51])([F:49])[F:50])[C:52]([F:53])([F:55])[F:54]
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참가 물질

7

반응물 5

HCID 6393Carbon tetrafluorideHCID 1216701,1,1,4,5,5,5-Heptafluoro-3-(pentafluoroethyl)-2,4-bis(trifluoromethyl)pent-2-eneHCID 522689Potassium Fluoride2회HCID 552549(Trifluoromethyl)trimethylsilane2회HCID 226420151,1,1,5,5,5-Hexafluoro-3-[1-(trifluoromethyl)-1,2,2,2-tetrafluoroethyl]-2,4,4-tris(trifluoromethyl)-2-pentene

생성물 1

HCID 73990785
Perfluoro 4,4-dimethyl-3-isopropyl-2-pentene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1 mmol (450 mg) of perfluoro(3-ethyl-2,4-dimethyl-2-pentene) and 4.0 mmol (568.8 mg) of trifluoromethyltrimethylsilane were weighed into a 10-ml fluororesin-made reaction container, then 1 ml of dimethyl formamide and 0.1 mmol of acidic potassium fluoride (KHF2, 7.8 mg) were added therein. A fluororesin-made magnetic stirrer was placed and the mixture was stirred vigorously for 1 hour at room temperature, and then 1.0 mmol of trifluoromethyltrimethylsilane (142.2 mg) and 0.1 mmol of acidic potassium fluoride (KHF2, 7.8 mg) were added and the mixture was further stirred vigorously for 1 hour at room temperature. After completion of the reaction, the transparent lower perfluorocarbon layer was analyzed by gas chromatography using a capillary column (NB-1, 0.25 μm, 1.5 mm ID×60 m). The yield of the main product perfluoro(2,4,4-trimethyl-3-isopropyl-2-pentene) was 74.5% by weight. As the by-product, perfluoro 4,4-dimethyl-3-isopropyl-2-pentene was obtained at the yield of 25.5% by weight. The starting material perfluoro(3-ethyl-2,4-dimethyl-2-pentene) was consumed completely by the reaction.

후처리

  1. customA fluororesin-made magnetic stirrer was placed
  2. stirringthe mixture was further stirred vigorously for 1 hour at room temperature
  3. customAfter completion of the reaction

출처 및 근거

ORD 기록
ord-13ce255a86bf4c28b9543ff9474bc153
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06710214B2

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