反応 #481612

反応方程式

potassium trifluoromethanesulfonate salt

acetone

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

diethyl ether

→

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

収率 87.8%

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   その他To the solution, a solution prepared
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   その他the 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
   その他the insoluble matter was removed by filtration
7. 7
   workup.DISTILLATIONChloroform in the filtrate was distilled off under reduced pressure
8. 8
   その他to obtain a transparent viscous liquid
9. 9
   ろ過The deposited white crystal was collected by filtration
10. 10
    その他recrystallized from ethyl acetate
11. 11
    その他The resulting white powder was dried under reduced pressure at 30° C. for six hours

実験手順

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%).

出典