関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 3',5'-Bis(trifluoromethyl)acetanilide | HCID 723600 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 1-Acetamido-2-nitro-3,5-bis(trifluoromethyl)benzene | HCID 19958574 | — |
反応手順
To a solution of 1-acetamido-3,5-bis(trifluoromethyl)benzene (400 mg, 1.37 mmol) in concentrated H2SO4 (3 mL) at 0° C. was added dropwise 70% HNO3 (0.4 mL, Baker). The mixture was stirred at 0° C. for 0.5 h, then at room temperature for 3 h and it was poured into ice water (10 g). The precipitate was collected by filtration, affording 400 mg of crude product which contained two compounds by 1H NMR. It was separated on a column of silica gel, eluted with chloroform, to afford 134 mg of pure 1-acetamido-2-nitro-3,5-bis(trifluoromethyl)benzene as white long needles. mp: 190°-2° C., 1H NMR (CDCl3): δ 2.226 (s, 3H), 7.765 (s, 1H), 7.978 (s, 1H); 8.918 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05620979 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-0efd3ef062964cf0acdd2fd1226f93bf |
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| 出典メモ | uspto-grants-1997_04 |
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