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

HRID 1443593노트

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HRID 1443593 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

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-f778d2aa96ea414db37098985e0b93c8
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662402B2

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