化工社化工社 化学情報印刷レポート · 研究参考用
2,5-Dimethylaniline → (4-Iodo-2,5-Dimethylphenyl)Amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dimethylaniline | HCID 7259 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Pyrosulfite | HCID 656671 | — |
| 反応物 | Trimethylbenzylammonium Dichloroiodate | HCID 56924451 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (4-Iodo-2,5-Dimethylphenyl)Amine | HCID 4770984 | — |
反応手順
25.0 g (71.8 mmol) of benzyltrimethylammonium dichloriodate and 12.8 g (92.5 mmol) of potassium carbonate are added to a solution of 8.8 ml of (70.8 mmol) of 2,5-dimethylaniline in 250 ml of methanol and 600 ml of dichloromethane and stirred for 1 hour at ambient temperature. Then the inorganic salts are suction filtered and the solvent is distilled off. The residue is combined with a solution of 13.5 g (70.8 mmol) of sodium pyrosulphite in 640 ml of water and extracted with ether. The combined organic extracts are dried over sodium sulphate and evaporated down. The crude product is triturated with petroleum ether, suction filtered and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06479524B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-31f9fcdb7d0f4fb996b038725fc7271d |
| 出典メモ | uspto-grants-2002_11 |