関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (E)-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-one | HCID 11110117 | — |
| 溶媒 | Dce dmf | HCID 20184825 | — |
| 生成物 | Diclopentezol | HCID 91738 | 63.8% |
反応手順
166 Milligrams (1.02 mmole) of the present compound obtained in Example 1 was dissolved in a 1,2-dichloroethane/dimethylformamide (27 ml/0.5 ml) mixed solvent, and 5 ml of a 1,2-dichloroethane solution containing 975 mg (3.0 mmoles) of (E)-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-one (E/Z=94.8/5.2) was added dropwise thereto. After reaction at room temperature for 16.5 hours, 2% hydrochloric acid was added to separate the reaction solution into an aqueous and organic layers. After concentrating the organic layer, the residue was purified by column chromatography on silica gel to obtain 624 mg of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-ol. The ratio of the E-form alcohol to Z-form alcohol was 93.8 to 6.2, and the enantiomer ratio of the E-form alcohol was: (+)-isomer: (-)-isomer=18:82.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04749809 |
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| 出典データセット | uspto-grants-1988_06 |
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| ORD ID | ord-a764cf831b50408cba4033516b0467d6 |
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| 出典メモ | uspto-grants-1988_06 |
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