Ethyl Acetate → 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium nonafluorobutanesulfonate

HRID 393501

Reaktionsgleichung

Reaktionsgleichung von HRID 393501
[F:1][C:2]([F:17])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:12])([F:11])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].[K+].[Br-].[O:20]=[C:21]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH2:22][S+:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1.C(OCC)(=O)C>O.CO>[F:17][C:2]([F:1])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:11])([F:12])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].[O:20]=[C:21]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH2:22][S+:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1

Komponenten

6

Edukt 3

HCID 8857Ethyl AcetateHCID 225645781-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromideHCID 23675274Potassium perfluorobutanesulfonate

Produkt 1

HCID 225645872-Oxo-3,3-dimethylbutyl-thiacyclopentanium nonafluorobutanesulfonateAusbeute 63,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

In a mixed solvent of 500 ml of water and 100 ml of methanol was dissolved 10 g of potassium perfluorobutanesulfonate, and to the solution was added a solution containing 7.75 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide dissolved in 50 ml of methanol. The aqueous solution was extracted twice with each 100 ml of chloroform, and the organic phase was washed with water and concentrated to obtain an oily product. To the oily product was added ethyl acetate, and the solution was again concentrated to obtain a solid product. The solid product was collected by filtration and subjected to reslurry with diisopropyl ether to obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.

Aufarbeitung

  1. additionto the solution was added a solution
  2. extractionThe aqueous solution was extracted twice with each 100 ml of chloroform
  3. washthe organic phase was washed with water
  4. concentrationconcentrated
  5. customto obtain an oily product
  6. concentrationthe solution was again concentrated
  7. customto obtain a solid product
  8. filtrationThe solid product was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-b67ff457c9c04f028399ffa57e7c4806
Quelldatensatz
uspto-grants-2004_10
Patentnummer
US06808862B2

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