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Triethylamine → 5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-2-(1-methoxycyclohexyloxy)methyl-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 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 | 5-(3,5-Dichlorophenylthio)-4-isopropyl-1-methyl-2-(1-methoxycyclohexyloxy)methyl-1H-imidazole | HCID 18792007 | 83.4% |
反応手順
To a solution of 5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-2-hydroxymethyl-1H-imidazole (14) (33 mg, 0.1 mmol) prepared in accordance with the method as described in WO 96/10019 and p-toluenesulfonic acid pyridinium (27.6 mg, 0.11 mmol) in toluene (1.5 mL) was added 1-methoxycyclohexene (112 mg, 1.00 mmol) under ice-cooling, and stirred at room temperature for 6 hours. 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 purified by chromatography on an alumina column (eluate: toluene) to give the compound 15 (37.0 mg, 70%) as oil. Rf 0.16 (Al2O3 60, Type E, toluene).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06054591 |
| 出典データセット | uspto-grants-2000_04 |
| ORD ID | ord-a286971f7e184e91b02b73dd4c884107 |
| 出典メモ | uspto-grants-2000_04 |