関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-Bromo-2-methoxybenzaldehyde | HCID 90684 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Bromo-2-methoxybenzonitrile | HCID 4418560 | — |
反応手順
A mixture of 5-Bromo-o-anisaldehyde (6.45 g), hydroxylamine hydrochloride (2.2 g), sodium acetate (4.1 g) and acetic acid (20 mL) was heated at 100 ° C. with stirring for 1 h. Acetic anhydride was added (20 mL) and the mixture was refluxed for 8 h. The reaction mixture was poured onto ice water and the mixture was made basic by the careful addition of 50% sodium hydroxide. The product was extracted with ether, the ether extracts were dried over magnesium sulfate and the sovent was removed in vacuo. The residue was crystallized from ether/hexane to afford 5-Bromo-2-methoxy-benzonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05646280 |
|---|
| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-b6043656dfe24c09833bc4f307bc72ed |
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| 出典メモ | uspto-grants-1997_07 |
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