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Hydrochloric Acid → HCID 86612543, Verbindung

HRID 1443557
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1443557
[F:1][C:2]([F:11])([F:10])[CH2:3][CH2:4][CH:5]([C:8]#[N:9])[C:6]#[N:7].[Cl:12][C:13]([F:21])([F:20])[C:14]([Cl:19])([F:18])[CH2:15][CH2:16]I.C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[Cl:19][C:14]([F:18])([C:13]([Cl:12])([F:21])[F:20])[CH2:15][CH2:16][C:5]([CH2:4][CH2:3][C:2]([F:10])([F:11])[F:1])([C:8]#[N:9])[C:6]#[N:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 47126711,2-dichloro-1,1,2-trifluoro-4-iodobutaneHCID 221857612-(3,3,3-Trifluoropropyl)malononitrile

Produkt 1

HCID 86612543HCID 86612543, VerbindungAusbeute 56,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679
Dimethyl Sulfoxide
Lösungsmittel

Versuchsvorschrift

1.6 g of 2-(3,3,3-trifluoropropyl)malononitrile and 3.1 g of 1,2-dichloro-4-iodo-1,1,2-trifluorobutane were dissolved in 5 ml of dimethyl sulfoxide, 1.4 g of potassium carbonate was added, and the mixture was stirred at room temperature for 6 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 1.9 g of 2-(3,4-dichloro-3,4,4-trifluorobutyl)-2-(3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (54)).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-f59b50bb07ec467ca2ead741fcf17772
Quelldatensatz
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07662402B2

Notizen zur Reaktion

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