関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitro-4-(trifluoromethyl)phenol | HCID 9816 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Amino-4-(trifluoromethyl)phenol | HCID 120246 | 83.3% |
反応手順
A mixture of 4-trifluoromethyl-2-nitrophenol(1.0 g, 4.8 mmol) and tin (II) chloride (5.4 g, 24.2 mmol) in ethanol(150 mL) was heated at 80° C. under argon. After 2 hours, the starting material had disappeared and the solution was allowed to cool down and then poured into ice. The pH was made slightly basic (pH7-8), by addition of solid NaOH, before being extracted with ethyl acetate. The organic phase was washed with brine, dried over MgSO4 and filtered. The solvent was evaporated and chromatography of the resulting solid on silica gel (4% MeOH/CH2Cl2) gave the desired product(708 mg, 83%). 1H NMR (CD3OD): d 6.87 (s, 1H), 6.80 (d, 1H), 6.69 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211373B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-69ca5bf0c43b45a5badc27606023348a |
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| 出典メモ | uspto-grants-2001_04 |
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