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Phenylhydrazine → 2-amino-4-nitro-N'-phenylbenzohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | 4-Nitro-isatoic anhydride | HCID 282089 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-amino-4-nitro-N'-phenylbenzohydrazide | HCID 49839975 | — |
反応手順
Into a 1000-mL 3-necked round-bottom flask, was placed a solution of 7-nitro-1H-benzo[d][1,3]oxazine-2,4-dione (56 g, 269.23 mmol, 1.00 equiv) in ethanol (500 mL), 1-phenylhydrazine (31.98 g, 296.11 mmol, 1.10 equiv). The resulting solution was heated to reflux for 5 min. The resulting mixture was then concentrated under vacuum. The residue was applied onto a silica gel column with dichloromethane/petroleum ether (1:2˜1:0) and ethyl acetate/petroleum ether (1:1) to yield 2-amino-4-nitro-N′-phenylbenzohydrazide as a yellow solid. MS: 273 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822447B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-5f75d9a26c594fa3ba5a2d32857f915a |
| 出典メモ | uspto-grants-2014_09 |