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1-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromide → 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium nonafluorobutanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 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 | 64.2% |
反応手順
Potassium perfluorobutanesulfonate (10 g) was dissolved in a mixed solvent comprising 500 ml of water and 100 ml of methanol, and a solution obtained by dissolving 7.7 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide in 50 ml of methanol was added to the above solution. The aqueous solution was extracted twice with 100 ml of chloroform, the organic phase was washed with water and concentrated, thereby an oily product was obtained. The above-obtained product was concentrated again with ethyl acetate, thereby a solid product was obtained. The solid product was filtered and re-slurried with diisopropyl ether, to thereby 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 | US06858370B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-71bd1248fad64cd58c8f6ed57ff96111 |
| 出典メモ | uspto-grants-2005_02 |