Potassium Trifluoromethanesulfonate → 2-Oxobutyl-thiacyclohexanium trifluoromethanesulfonate

HRID 394426

Reaktionsgleichung

Reaktionsgleichung von HRID 394426
[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[K+].[Br-].[O:11]=[C:12]([CH2:20][CH3:21])[CH2:13][S+:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>C(#N)C>[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[O:11]=[C:12]([CH2:20][CH3:21])[CH2:13][S+:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

Komponenten

4

Edukt 2

HCID 23664779Potassium TrifluoromethanesulfonateHCID 857879522-Oxobutyl-thiacyclohexanium bromide

Produkt 1

HCID 865848882-Oxobutyl-thiacyclohexanium trifluoromethanesulfonateAusbeute 75,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

In a 300 ml three-necked flask, 2 g of 2-oxobutyl-thiacyclohexanium bromide obtained in Example 1 was dissolved in 10 ml of acetonitrile. To the solution, a solution prepared by dissolving 1.5 g of a potassium trifluoromethanesulfonate salt in 100 ml of acetonitrile was added dropwise. After stirring for three hours, the deposited potassium bromide was removed by filtration and acetonitrile was distilled off under reduced pressure by an evaporator. The residue was dissolved in chloroform and the insoluble matter was removed by filtration. Chloroform in the filtrate was distilled off under reduced pressure and the residue (transparent viscous liquid) was cooled in a refrigerator at −20° C. for three hours. The residue was converted into a white crystal by cooling. The white crystal was recrystallized from ethyl acetate and then dried under reduced pressure at 30° C. for six hours to obtain 1.92 g of 2-oxobutyl-thiacyclohexanium trifluoromethanesulfonate (yield: 75.4%).

Aufarbeitung

  1. customTo the solution, a solution prepared
  2. additionwas added dropwise
  3. customthe deposited potassium bromide was removed by filtration and acetonitrile
  4. distillationwas distilled off under reduced pressure by an evaporator
  5. dissolutionThe residue was dissolved in chloroform
  6. customthe insoluble matter was removed by filtration
  7. distillationChloroform in the filtrate was distilled off under reduced pressure
  8. temperatureby cooling
  9. customThe white crystal was recrystallized from ethyl acetate
  10. customdried under reduced pressure at 30° C. for six hours

Quellen und Nachweise

ORD-Eintrag
ord-c43beca40851441bb27bd06eadff3021
Quelldatensatz
uspto-grants-2003_08
Patentnummer
US06602647B2

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