関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | 1-Methoxycyclohexene | HCID 70264 | — |
| 反応物 | (5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl)methanol | HCID 473916 | — |
| 反応物 | Pyridinium.p-toluenesulfonate | HCID 22033616 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(Cyclohexen-1-yloxy)methyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole | HCID 18791989 | 30% |
反応手順
The compound 14 (166 mg, 0.5 mmol), 1-methoxycyclohexene (280 mg, 2.50 mmol) and p-toluenesulfonic acid pyridinium (132 mg, 0.505 mmol) was dissolved in toluene (4 mL). The reaction mixture was stirred at room temperature for 20 hours. Benzene (60 mL) was added thereto, the reaction mixture was heated under reflux over 45 minutes and concentrated to a small amount. A drop of triethylamine was added to the reaction mixture, and the mixture was filtered to remove the insoluble matter. The filtrate was concentrated under reduced pressure. The residue was extracted with hexane, and filtered off the insoluble matter. The filtrate was purified by chromatography on an alumina column (eluate: toluene) to give the compound 17 (61 mg, 30%) as crystals. Mp 69-71° C. Rf 0.57 (Al2O3 60, Type E, toluene).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06054591 |
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| 出典データセット | uspto-grants-2000_04 |
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| ORD ID | ord-36badcf1f3224d059e74dd51e7602ed3 |
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| 出典メモ | uspto-grants-2000_04 |
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