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Hydrochloric Acid → 2-(2,2,3,3,4,4,4-Heptafluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile

HRID 1443578
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HRID 1443578 반응식
[F:1][C:2]([F:18])([C:9]([F:17])([F:16])[C:10]([F:15])([F:14])[CH:11]([F:13])[F:12])[CH2:3][CH:4]([C:7]#[N:8])[C:5]#[N:6].FC(F)(F)S(O[CH2:25][C:26]([F:35])([F:34])[C:27]([F:33])([F:32])[C:28]([F:31])([F:30])[F:29])(=O)=O.C(=O)([O-])[O-].[K+].[K+].Cl>COCCOC>[F:34][C:26]([F:35])([C:27]([F:32])([F:33])[C:28]([F:29])([F:31])[F:30])[CH2:25][C:4]([CH2:3][C:2]([F:18])([F:1])[C:9]([F:16])([F:17])[C:10]([F:14])([F:15])[CH:11]([F:13])[F:12])([C:7]#[N:8])[C:5]#[N:6]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 27748941H,1H-Heptafluorobutyl trifluoromethanesulphonateHCID 25242027(2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile

생성물 1

HCID 159796632-(2,2,3,3,4,4,4-Heptafluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile수율 3%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile and 3.3 g of 2,2,3,3,4,4,4-heptafluorobutyl trifluoromethanesulfonate were dissolved in 10 ml of ethylene glycol dimethyl ether, 0.97 g of potassium carbonate was added, and the mixture was stirred at room temperature for 7 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.07 g of 2-(2,2,3,3,4,4,4-heptafluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile (hereinafter, referred to as the present compound (79)).

후처리

  1. extractionfollowed by extraction with methyl tert-butyl ether
  2. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8d569b96c41147babf2a1d6e999d6326
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662402B2

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