化工社化工社 化学情報印刷レポート · 研究参考用
Melatonin → Melatonin Impurity 3
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Melatonin | HCID 896 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Melatonin Impurity 3 | HCID 832313 | 50% |
反応手順
Acetic anhydride (7 ml) is added with stirring to melatonin (500 mg) dissolved in benzene (50 ml). The mixture is heated for 72 h in refluxing benzene. The solvent is evaporated off and the crude product is taken up in water and then neutralized with sodium carbonate solution (pH>8). After extraction (dichloromethane), washing (water) and drying (magnesium sulphate), the crude product is flash-chromatographed (EtOAc eluent). N-[2-(5-Methoxyindol-3-yl)ethyl]diacetamide (4) (300 mg, 50% yield) is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06140372 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-8a236f1593674321bb6c343b8c23bcb0 |
| 出典メモ | uspto-grants-2000_10 |