Water → 2-(2,2,3,4,4,4-Hexafluorobutyl)malononitrile

HRID 1443591ノート

反応式

HRID 1443591 の反応式
FC(F)(F)S(O[CH2:7][C:8]([F:16])([F:15])[CH:9]([F:14])[C:10]([F:13])([F:12])[F:11])(=O)=O.C(=O)([O-])[O-].[K+].[K+].[C:25](#[N:29])[CH2:26][C:27]#[N:28].O>CS(C)=O>[F:15][C:8]([F:16])([CH:9]([F:14])[C:10]([F:13])([F:12])[F:11])[CH2:7][CH:26]([C:25]#[N:29])[C:27]#[N:28]

参加物

6

反応物 4

HCID 962WaterHCID 8010MalononitrileHCID 11430Potassium CarbonateHCID 588790322,2,3,4,4,4-Hexafluorobutyl trifluoromethanesulfonate

生成物 1

HCID 866125382-(2,2,3,4,4,4-Hexafluorobutyl)malononitrile収率 34.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

8.0 g of 2,2,3,4,4,4-hexafluorobutyl trifluoromethanesulfonate was dissolved in 15 ml of dimethyl sulfoxide, and 6.9 g of potassium carbonate was added. 5.0 g of malononitrile dissolved in 15 ml of dimethyl sulfoxide was added dropwise thereto, and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured to water and then extracted with diethyl ether. The organic layer was washed successively with water 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 2.0 g of 2-(2,2,3,4,4,4-hexafluorobutyl)malononitrile.

後処理

  1. additionwas added dropwise
  2. extractionextracted with diethyl ether
  3. washThe organic layer was washed successively with water and aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ddbd3d1c4477408fb7b939e626d48f80
出典データセット
uspto-grants-2010_02
特許番号
US07662402B2

反応ノート

読み込み中…