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1-Nitro-4-(2,2,2-trifluoroethoxy)benzene → 4-(2,2,2-Trifluoroethoxy)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Nitro-4-(2,2,2-trifluoroethoxy)benzene | HCID 2775769 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(2,2,2-Trifluoroethoxy)aniline | HCID 2777119 | 94.7% |
反応手順
1-Nitro-4-(2,2,2-trifluoroethoxy)benzene (5.5 g) was dissolved in methanol (100 ml), 10% palladium/activated carbon (50% in water, 2.5 g) was added thereto, and the mixture was stirred at room temperature for 24 hr under a hydrogen atmosphere. The palladium/activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure to give a dark orange oil residue. The obtained residue was dissolved in ethyl acetate (200 ml), and the solution was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained dark orange oil residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.5 g) as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09023858B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-2a6120c365e848ea9e2a60e59fb32e8b |
| 出典メモ | uspto-grants-2015_05 |