Hydrochloric Acid → (2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile

HRID 1443593ノート

反応式

HRID 1443593 の反応式
[F:1][C:2]([F:21])([C:12]([F:20])([F:19])[C:13]([F:18])([F:17])[CH:14]([F:16])[F:15])[CH2:3]OS(C(F)(F)F)(=O)=O.[C:22](#[N:26])[CH2:23][C:24]#[N:25].C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[F:21][C:2]([F:1])([C:12]([F:19])([F:20])[C:13]([F:17])([F:18])[CH:14]([F:15])[F:16])[CH2:3][CH:23]([C:22]#[N:26])[C:24]#[N:25]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 11430Potassium CarbonateHCID 27758912,2,3,3,4,4,5,5-Octafluoropentyl trifluoromethanesulfonate

生成物 1

HCID 25242027(2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile収率 18.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

15 g of (2,2,3,3,4,4,5,5-octafluoropentyl)trifluoromethanesulfonic acid and 2.6 g of malononitrile were dissolved in 20 ml of dimethyl sulfoxide, 5.5 g of potassium carbonate was added, and the mixture was stirred in a water bath for 3 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 2.0 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile.

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-f778d2aa96ea414db37098985e0b93c8
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…