Hydrochloric Acid → 2,2-Bis(2,2,3,4,4,4-hexafluorobutyl)malononitrile

HRID 1443587ノート

反応式

HRID 1443587 の反応式
[F:1][C:2]([F:15])([CH:9]([F:14])[C:10]([F:13])([F:12])[F:11])[CH2:3][CH:4]([C:7]#[N:8])[C:5]#[N:6].FC(F)(F)S(O[CH2:22][C:23]([F:31])([F:30])[CH:24]([F:29])[C:25]([F:28])([F:27])[F:26])(=O)=O.C(=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O>[F:1][C:2]([F:15])([CH:9]([F:14])[C:10]([F:12])([F:13])[F:11])[CH2:3][C:4]([CH2:22][C:23]([F:31])([F:30])[CH:24]([F:29])[C:25]([F:28])([F:27])[F:26])([C:7]#[N:8])[C:5]#[N:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 588790322,2,3,4,4,4-Hexafluorobutyl trifluoromethanesulfonateHCID 866125382-(2,2,3,4,4,4-Hexafluorobutyl)malononitrile

生成物 1

HCID 866125712,2-Bis(2,2,3,4,4,4-hexafluorobutyl)malononitrile収率 1.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

In 50 ml of acetone, 2.0 g of 2-(2,2,3,4,4,4-hexafluorobutyl)malononitrile and 5.3 g of 2,2,3,4,4,4-hexafluorobutyl trifluoromethanesulfonate were dissolved, 1.9 g of potassium carbonate was added and the mixture was stirred at room temperature for 10 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture and the mixture was extracted with t-butyl methyl 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 0.05 g of 2,2-bis(2,2,3,4,4,4-hexafluorobutyl)malononitrile (hereinafter, referred to as the present compound (95)).

後処理

  1. extractionthe mixture was extracted with t-butyl methyl 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-1345aecfa3a44cb683da51e10c225436
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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