関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | [(1R)-1-[(2R)-2-(2,4-Difluorophenyl)-2-oxiranyl]ethyl]3,5-dinitrobenzoate | HCID 10691998 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (1R)-1-[(2R)-2-(2,4-difluorophenyl)-2-oxiranyl]ethanol | HCID 10536015 | 98.5% |
反応手順
[(1R)-1-[(2R)-2-(2,4-Difluorophenyl)-2-oxiranyl]ethyl] 3,5-dinitrobenzoate (50 g) was dissolved in methanol (2 liters). To the solution was added dropwise 1N sodium hydroxide aqueous solution (255 ml) at room temperature. The mixture was stirred for an hour at room temperature and neutralized with 1N hydrochloric acid (127 ml). Methanol was distilled off under reduced pressure. To the residue were added ethyl acetate (1liter) and water (200 ml). The mixture was extracted with ethyl acetate. The organic layer was washed with saturated saline (200 ml), dried over magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1:3) to give (1R)-1-[(2R)-2-(2,4-difluorophenyl)-2-oxiranyl] ethanol (25 g) as a pale yellow oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05371100 |
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| 出典データセット | uspto-grants-1994_12 |
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| ORD ID | ord-4dbea9fd49384f92855df76c4b98af8b |
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| 出典メモ | uspto-grants-1994_12 |
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