化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus oxide (P4O10) → 2-Bromo-4-methylbenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | 2-Bromo-4-methylbenzamide | HCID 262340 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Bromo-4-methylbenzonitrile | HCID 820802 | 98.2% |
反応手順
To a suspension of 2-bromo-4-methylbenzamide (14.8 g, 69.1 mmol) in CHCl3 was added phosphorous pentoxide (24.5 g, 172.8 mmol) and the mixture keep refluxing for 12 h. The reaction was allowed to cool to room temperature, and put into the ice water under the condition of stirring. The organic layer was separated and the aqueous layer was extracted with CHCl3 (150 mL×2). The combined organic phase was washed with brine, and dried over Na2SO4. Evaporation of the solvent afforded the title compound, 2-bromo-4-methylbenzonitrile (13.3 g, 98%). 1H NMR (400 MHz, CDCl3): δ 2.41 (s, 3 H), 7.20 (d, J=8.0 Hz, 1 H), 7.51-7.54 (m, 2 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067408B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-b6583c8a462e4d31a2e5ff9461ca532b |
| 出典メモ | uspto-grants-2011_11 |