関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | 2-Benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(pyridin-4-yl)methyl-1H-imidazole | HCID 9848752 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | {5-[(3,5-Dichlorophenyl)sulfanyl]-4-isopropyl-1-((pyridin-4-YL)methyl)imidazol-2-YL}methanol | HCID 9844329 | — |
反応手順
To the compound (6) was added concentrated aqueous hydrochloric acid (50 ml). The mixture was heated at 90° C. for 2 hours and then cooled down. To the mixture were added water (50 ml) and toluene (20 ml). The aqueous layer was separated and neutralized by 30% aqueous sodium hydroxide. The compound (12) was extracted with ethyl acetate (50 ml), and the ethyl acetate layer was washed with water (30 ml). Each aqueous layer was extracted with ethyl acetate (20 ml). The ethyl acetate layer was collected and concentrated under reduced pressure to yield oily residue. To the oily residue was slowly added diisopropyl ether (50 ml) for crystallization. The obtained slurry was stirred at room temperature for 30 minutes, filtered, washed with diisopropyl ether (30 ml) and dried to yield the compound (12) (10.4 g) as a white crystal. Yield from the compound (22):82%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087764B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-b9dca31d80aa4786984f28cacece28d0 |
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| 出典メモ | uspto-grants-2006_08 |
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