関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Hexane, 2,5-dichloro-2,5-dimethyl- | HCID 80360 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloride methane | HCID 20976018 | — |
| 生成物 | 5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol | HCID 268786 | 90.8% |
反応手順
To a mixture of aluminum trichloride (3.0 g, 22.5 mmol), dichloromethane (50 ml) and 2,5-dichloro-2,5-dimethylhexane (15.0 g, 81.9 mmol) is added dropwise into a solution of phenol (7.7 g, 81.90 mmol) in 50 ml of methane dichloride, then the reaction mixture is heated for 4 hours at 35° C. After cooled, the reaction mixture is poured into ice (200 g) and extracted with ether (3×80 ml). The organic phase is washed with 10% NaHCO3 solution (2×150 ml), dried over MgSO4 and evaporated to give a crude product, which is crystallized from ethanol to give the title compound (15.20 g, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07192970B2 |
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| 出典データセット | uspto-grants-2007_03 |
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| ORD ID | ord-3d0d8ee35d8947cebc541e6f02e65792 |
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| 出典メモ | uspto-grants-2007_03 |
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