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HRID 1005508作成日:2026年10月25日
Toluene → 1-[2-(Cyclohexen-1-yloxy)ethoxymethyl]-5-(3,5-dimethylphenylthio)-4-isopropyl-2-methyl-1H-imidazole
https://huagongshe.com/reaction/1005508
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-Methoxycyclohexene | HCID 70264 | — |
| 反応物 | 2-[5-(3,5-Dimethyl-phenylsulfanyl)-4-isopropyl-2-methyl-imidazol-1-ylmethoxy]-ethanol | HCID 478180 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[2-(Cyclohexen-1-yloxy)ethoxymethyl]-5-(3,5-dimethylphenylthio)-4-isopropyl-2-methyl-1H-imidazole | HCID 18792037 | 75% |
反応手順
A solution of the compound 1 (33.4 mg, 0.1 mmol) and p-toluenesulfonic acid hydrate (20.0 mg, 0.105 mmol) in a mixture of methylene chloride (1 mL) - toluene (0.1 mL) was concentrated under reduced pressure. The residue was dissolved in a mixture of dioxane (2 mL) - benzene (0.5 mL), to which was added 1-methoxycyclohexene (112 mg, 1.00 mmol). The reaction mixture was heated under reflux, and concentrated to a small volume over 1 hour. A drop of triethylamine was added to the reaction mixture, and the mixture was concentrated under reduced pressure. Hexane was added to the residue, the mixture was filtered to remove the insoluble matter, and the filtrate was purified by chromatography on an alumina column (eluate: hexane - ethyl acetate (2:1)) to give the same compound 6 (31 mg, 75%) as oil. Rf 0.62 (Al2O3 60, Type E, 2:1 hexane -EtOAc).
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-44cf4febb0354ec187e3d5f7e36ddeaa |
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| 出典メモ | uspto-grants-2000_04 |
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