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p-Toluenesulfonic acid → 1-Phenylcyclohexene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1-Phenylcyclohexanol | HCID 15319 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Phenylcyclohexene | HCID 13043 | — |
反応手順
1-phenylcyclohexan-1-ol (24.9 mmol), p-toluenesulfonic acid (500 mg) and toluene (200 mL) are mixed together in a 500 mL 3 neck flask fitted with a thermometer and Dean Stark trap and stirred at reflux for 4 hours under a nitrogen atmosphere. The reaction is then allowed to cool to room temperature and concentrated under reduced vacuum. The crude material is then taken into methylene chloride, washed once with water, dried over potassium carbonate, filtered, and concentrated under reduced vacuum. This material can then be purified via silica gel chromatography employing the Water's Prep 2000 and eluting with a solvent of hexane/methylene chloride 9:1 to yield the intermediate title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06900353B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-9e5954cfd69347868396b871719b57fe |
| 出典メモ | uspto-grants-2005_05 |