関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tert-Butylbenzene | HCID 7366 | — |
| 反応物 | Iodosylbenzene | HCID 92125 | — |
| 反応物 | 1-Propanesulfonic acid, 1,1,2,3,3,3-hexafluoro- | HCID 9794628 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 22625489 | HCID 22625489 | — |
反応手順
4.4 g (20 mmol) of iodosylbenzene was suspended in 100 ml of dry dichloromethane. The suspension was cooled to 0° C. with stirring. 4.65 g (20 mmol) of 3,3,3,2,1,1-hexafluoropropane sulfonic acid (optionally distilled) was added at the same temperature thereto under exclusion of moisture. The mixture was stirred at room temperature for 3 hours. The temperature of the mixture was returned to 0° C., and 2.68 g (20 mmol) of 4-t-butylbenzene was added thereto at that temperature. The temperature of the mixture was returned to room temperature, followed by stirring for 6 hours. Thereafter, the insolubles were removed by filtration. The solvent was removed from the filtrate. The oily residue was purified by recrystallization (twice) from diethyl ether. The structure was confirmed by 1H-NMR (CDCl3): δ=0.81 (s, 9H), 4.98-5.22 (m[d], 1H), 7.18-7.23 (d, 2H), 7.58-7.65 ppm (m, 7H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06358665B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-10b1fad91dc64ce68db68fd3e18524a1 |
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| 出典メモ | uspto-grants-2002_03 |
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