関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Trifluoromethanesulfonate | HCID 23664779 | — |
| 反応物 | 2-Oxobutyl-thiacyclohexanium bromide | HCID 85787952 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Oxobutyl-thiacyclopentanium trifluoromethanesulfonate | HCID 86584890 | 69.8% |
反応手順
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 1.6 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 1.7 g of 2-oxobutyl-thiacyclopentanium trifluoromethanesulfonate (yield: 65.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06602647B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-1292fc0bf1b9431fa40cdfb82ef84c80 |
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| 出典メモ | uspto-grants-2003_08 |
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