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

HRID 1443580ノート

反応式

HRID 1443580 の反応式
[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:34])([F:33])[CH:27]([F:32])[C:28]([F:31])([F:30])[F:29])(=O)=O.C(=O)([O-])[O-].[K+].[K+].Cl>COCCOC>[F:33][C:26]([F:34])([CH:27]([F:32])[C:28]([F:31])([F:30])[F:29])[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 25242027(2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrileHCID 588790322,2,3,4,4,4-Hexafluorobutyl trifluoromethanesulfonate

生成物 1

HCID 866125642-(2,2,3,4,4,4-Hexafluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile収率 2.7%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile and 3.1 g of 2,2,3,4,4,4-hexafluorobutyl 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 0.06 g of 2-(2,2,3,4,4,4-hexafluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile (hereinafter, referred to as the present compound (81)).

後処理

  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

出典と根拠

ORDレコード
ord-2706cab04c864f989a3b0e4cfb207088
出典データセット
uspto-grants-2010_02
特許番号
US07662402B2

反応ノート

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