関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Nitro-2,5-bis(trifluoromethyl)benzene | HCID 2734048 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2,5-Bis(trifluoromethyl)aniline | HCID 719818 | 73% |
反応手順
Into an autoclave, 1.05 g of Raney Nickel catalyst (10 wt %) and 100 ml of isopropanol were introduced, and 10.0 g of 2,5-bis(trifluoromethyl)nitrobenzene was added thereto in small amounts. Hydrogen gas was blown until 5 kg/cm2 with stirring, and the temperature was increased to 70° C. Reaction was carried out at from 70 to 90° C. for 8 hours. After the temperature was recovered to room temperature, hydrogen gas was evacuated, and the Raney Nickel was subjected to filtration and washed with isopropanol. The solvent was concentrated to obtain 2,5-bis(trifluoromethyl)aniline (6.42 g, yield 73%, purity by GC 99.4%). As a result of analysis by GC-Mass, 1H-NMR and 19F-NMR, the product was confirmed to be 2,5-bis(trifluoromethyl)aniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06930214B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-8eb358c7da34435c913e5460880d5ac0 |
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| 出典メモ | uspto-grants-2005_08 |
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