化工社化工社 化学情報印刷レポート · 研究参考用
Aniline → 2-Norbornylphenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Bicyclo(2.2.1)heptan-2-one | HCID 10345 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | HCID 178418385 | HCID 178418385 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 2-Norbornylphenylamine | HCID 54125158 | 106.9% |
反応手順
In a 250 mL flask equipped with a Dean-Start separator, the following mixture is brought to reflux: 9.3 g of aniline, 12.1 g 2-norbornanone, 13.2 g benzotriazole and 120 mL xylene. After 16 h, the mixture is reduced to dryness, then it is solubilized in 300 mL methanol, and the product is reduced with 6 g NaBH4 at 50° C. for 1 h. The mixture is then poured into 200 mL water and the organic product is extracted with 3×100 mL toluene. The organic phase is recovered, dried over magnesium sulfate, and then reduced to dryness. In this manner, 20 g of the desired amine are produced.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06030555 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-cae0fbda27d04fde94c95b484282019f |
| 出典メモ | uspto-grants-2000_02 |