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Ethyl Acetate → 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium nonafluorobutanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromide | HCID 22564578 | — |
| 反応物 | Potassium perfluorobutanesulfonate | HCID 23675274 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium nonafluorobutanesulfonate | HCID 22564587 | 63.8% |
反応手順
In a mixed solvent of 500 ml of water and 100 ml of methanol was dissolved 10 g of potassium perfluorobutanesulfonate, and to the solution was added a solution containing 7.75 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide dissolved in 50 ml of methanol. The aqueous solution was extracted twice with each 100 ml of chloroform, and the organic phase was washed with water and concentrated to obtain an oily product. To the oily product was added ethyl acetate, and the solution was again concentrated to obtain a solid product. The solid product was collected by filtration and subjected to reslurry with diisopropyl ether to obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06808862B2 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-b67ff457c9c04f028399ffa57e7c4806 |
| 出典メモ | uspto-grants-2004_10 |