HuagongsheHuagongshe Chemistry Print Report · For research reference only
Melatonin → Melatonin Impurity 3
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Melatonin | HCID 896 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | Melatonin Impurity 3 | HCID 832313 | 50% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06140372 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-8a236f1593674321bb6c343b8c23bcb0 |
| Source note | uspto-grants-2000_10 |