참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetone | HCID 180 | — |
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | 1-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromide | HCID 22564578 | — |
| 반응물 | Potassium Trifluoromethanesulfonate | HCID 23664779 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate | HCID 18175940 | 87.8% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06602647B2 |
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| 출처 데이터셋 | uspto-grants-2003_08 |
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| ORD ID | ord-95bef059a97f4998bf22597655fbac5c |
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| 출처 메모 | uspto-grants-2003_08 |
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