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Hydrochloric Acid → HCID 86612553, 화합물

HRID 1443567
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HRID 1443567 반응식
[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].[Cl:19][C:20]([F:28])([F:27])[C:21]([Cl:26])([F:25])[CH2:22][CH2:23]I.C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[Cl:26][C:21]([F:25])([C:20]([Cl:19])([F:28])[F:27])[CH2:22][CH2:23][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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 47126711,2-dichloro-1,1,2-trifluoro-4-iodobutaneHCID 25242027(2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile

생성물 1

HCID 86612553HCID 86612553, 화합물수율 2.2%

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

실험 절차

1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile and 1.5 g of 1,2-dichloro-4-iodo-1,1,2-trifluorobutane were dissolved in 5 ml of dimethyl sulfoxide, 0.83 g of potassium carbonate was added, and the mixture was stirred at room temperature for 9 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 0.05 g of 2-(3,4-dichloro-3,4,4-trifluorobutyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile (hereinafter, referred to as the present compound (67)).

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-4c47e19b76ea4271865fea92c4e05633
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662402B2

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