化工社化工社 化学情報印刷レポート · 研究参考用
Water → Benzenemethanamine, 3-chloro-4-methyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Chloro-p-toluonitrile | HCID 88894 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzenemethanamine, 3-chloro-4-methyl- | HCID 106225 | 84.7% |
反応手順
15 ml solution of 2.0 g 3-chloro-4-methylbenzonitrile in tetrahydrofuran was added dropwise into 40 ml solution of 453 mg lithium aluminum hydride in tetrahydrofuran in a nitrogen atmosphere. The mixture was heated under reflux for 2 hr and 10 min. The mixture was ice-cooled, and 0.45 ml water, 0.45 ml of 15% aqueous sodium hydroxide, and 1.35 ml water were added dropwise thereinto such that the solution was kept at 10° C. or less. The solution was filtered through Celite, and the resulting filtrate was dried by adding anhydrous sodium sulfate. It was filtered through a NH-form silica gel, and the filtrate was evaporated to give 1.74 g of 3-chloro-4-methylbenzylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699870B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-e5378e02f93a445b938ba075683e10be |
| 出典メモ | uspto-grants-2004_03 |