関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Methyl (2S)-2-(2,3,4-trifluoroanilino)propionate | HCID 10125210 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | (2S)-2-(2,3,4-Trifluoroanilino)propanol | HCID 11401466 | 84.1% |
反応手順
Under ice-cooling, sodium borohydride (1.2 g) was dissolved in IPA (50 ml). After adding methanol (5 ml), a solution of the compound (5.0 g) obtained in Example 1 in IPA was dropped therein to. Then the liquid reaction mixture was heated to 50° C. and stirred for 1 hour. Next, hydrochloric acid (1 mol/l) was added and the mixture was stirred for a while. Then a saturated aqueous solution of sodium hydrogencarbonate was added and the mixture was extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate and filtered. After evaporating the solvent, the obtained residue was subjected to silica gel column chromatography to give 3.7 g (84%) of the title compound as an oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087778B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-5d5a9bdc3c81411cb148de996528a9c6 |
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| 出典メモ | uspto-grants-2006_08 |
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