Reaktion #481612

Reaktionsgleichung

potassium trifluoromethanesulfonate salt

acetone

2-oxo-3,3-dimethylbutyl-thiacyclopentanium bromide

diethyl ether

→

2-oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate

Ausbeute 87.8%

Lösungsmittel

acetonitrile

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo the solution, a solution prepared
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   Sonstigethe deposited potassium bromide was removed by filtration and acetonitrile
4. 4
   workup.DISTILLATIONwas distilled off under reduced pressure by an evaporator
5. 5
   workup.DISSOLUTIONThe residue was dissolved in chloroform
6. 6
   Sonstigethe insoluble matter was removed by filtration
7. 7
   workup.DISTILLATIONChloroform in the filtrate was distilled off under reduced pressure
8. 8
   Sonstigeto obtain a transparent viscous liquid
9. 9
   FiltrationThe deposited white crystal was collected by filtration
10. 10
    Sonstigerecrystallized from ethyl acetate
11. 11
    SonstigeThe resulting white powder was dried under reduced pressure at 30° C. for six hours

Vorschrift

In a 300 ml three-necked flask, 2 g of 2-oxo-3,3-dimethylbutyl-thiacyclopentanium bromide obtained in Example 1 was dissolved in 20 ml of acetonitrile. To the solution, a solution prepared by dissolving 1.69 g of a potassium trifluoromethanesulfonate salt in 50 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 to obtain a transparent viscous liquid. To the transparent viscous liquid, 5 ml of acetone was added and the solution was added dropwise to 300 ml of diethyl ether. The deposited white crystal was collected by filtration and then recrystallized from ethyl acetate. The resulting white powder was dried under reduced pressure at 30° C. for six hours to obtain 2.21 g of 2-oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate (yield: 87.7%).

Quelle