関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Bromo-5-fluoro-2-methyl-3-nitrobenzene | HCID 2773385 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 3-Bromo-5-fluoro-2-methylaniline | HCID 2737641 | — |
反応手順
To iron powder (325 mesh, 2.25 g, 40.3 mmol) in 30 ml water and 80 ml isopropanol was added commercially available 1-bromo-5-fluoro-2-methyl-3-nitro-benzene (3.04 g, 13 mmol) in 45 ml isopropanol and NH4Cl (1.46 g, 27.3 mmol). The resulting mixture was heated at 110° C. for 2 h. After evaporation of most of the isopropanol the aq solution was extracted with ethyl acetate three times. The combined organic layers were washed with water and brine, dried over MgSO4, filtered and evaporated. The crude product was used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08378092B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-e6322d2c07c0442eb0a7e6b983a5a71a |
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| 出典メモ | uspto-grants-2013_02 |
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