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Hydrochloric Acid → HCID 86642965, Verbindung

HRID 888642
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 888642
C1(C)C=CC(S([O:10][CH2:11][CH2:12][C:13]([F:25])([F:24])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])(=O)=O)=CC=1.[C:27]([O-])(=[S:29])[CH3:28].[K+].Cl>CN(C)C=O>[C:27]([O:10][CH2:11][CH2:12][C:13]([F:24])([F:25])[C:14]([F:22])([F:23])[C:15]([F:20])([F:21])[C:16]([F:17])([F:18])[F:19])(=[S:29])[CH3:28]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 23670855Potassium ethanethioateHCID 866429663,3,4,4,5,5,6,6,6-Nonafluorohexyl 4-methylbenzene-1-sulfonate

Produkt 1

HCID 86642965HCID 86642965, VerbindungAusbeute 57,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 42.65 g of 3,3,4,4,5,5,6,6,6-nonafluorohexyl p-toluenesulfonate, 100 ml of N,N-dimethylformamide and 11.65 g of potassium thioacetate was heated and stirred at 80° C. for 4 hours under a nitrogen atmosphere. A reaction vessel was cooled in an ice bath. To the reaction mixture was added an aqueous 1N hydrochloric acid solution, and the mixture was extracted with 200 ml of ethylacetate twice. Organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over sodium sulfate, filtered, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 18.91 g of 3,3,4,4,5,5,6,6,6-nonafluorohexyl thioacetate represented by the formula:

Aufarbeitung

  1. temperaturewas heated
  2. temperatureA reaction vessel was cooled in an ice bath
  3. extractionthe mixture was extracted with 200 ml of ethylacetate twice
  4. washwashed with an aqueous saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-07e0b8b6ba364377a58e751349812a6d
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08247596B2

Notizen zur Reaktion

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