関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | n-[4-Chloro-3-(trifluoromethyl)phenyl]acetamide | HCID 67676 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | N-[4-Chloro-2-nitro-5-(trifluoromethyl)phenyl]acetamide | HCID 22318004 | 91% |
反応手順
To 3-acetamido-6-chlorobenzotrifluoride (908 mg, 3.82 mmol) in concentrated H2SO4 (4 mL) at 0° C. was added dropwise 70% HNO3 (0.5 mL, Baker). The mixture was stirred at 0° C. for 0.5 h, then at room temperature 3 h, and it was poured into ice water (15 g). The precipitate was collected by filtration, affording 990 mg (91%) of crude 3-acetamido-6-chloro-4-nitrobenzotrifluoride. It was crystallized from EtOH/H2O to give 770 mg of pure compound as yellow needles. 1H NMR (CDCl3): δ2.326 (s, 3H), 8.345 (s, 1H), 9.293 (s, 1H), 10.222 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05622952 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-33cc602ac41342cb9e5ad6e79081599a |
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| 出典メモ | uspto-grants-1997_04 |
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