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3-Aminobenzamide → 3-Nitrosobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Aminobenzamide | HCID 1645 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Nitrosobenzamide | HCID 1679 | 34% |
反応手順
To a stirred solution of 3-aminobenzamide (Aldrich Chemical Co.) (0.476 g, 3.50 mmol) in ethyl acetate (50 ml) at ambient temperature was added 1.208 g of 3-chloroperoxybenzoic acid (commercial grade, 50-60% purity, Aldrich), whereupon the solution turned green. After 10 minutes the mixture was extracted with 0.14M aqueous sodium bicarbonate (58 ml), washed with three successive 40-ml portions of water, dried over sodium sulfate, then reduced in volume to 20 mL by rotary evaporation and placed in the freezer (-20° C.), whereupon the product slowly deposited as a light yellow solid daring a period of 72 hours (0.180 g, 34% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05753674 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-f4cc50c106fd4a8d8050cae5f25fe510 |
| 出典メモ | uspto-grants-1998_05 |