HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59216604, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 59216597 | HCID 59216597 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59216604 | HCID 59216604 | — |
Reaction Steps
5-Amino-3-hydroxy-3,4-dihydroquinolin-2(1H)-one (300 mg, 1.68 mmol) is dissolved in THF (10 ml) and slowly added to a refluxing mixture of LiAlH4 (319 mg, 8.42 mmol) in 8 ml THF under an argon atmosphere. After 30 min refluxing the mixture is cooled to room temperature, ethyl acetate (10 ml) is added cautiously, thereafter water is added slowly and cautiously until a light grey precipitate formed. The solvent is collected and the precipitate is washed several times with ethyl acetate, the combined organic extracts are washed with water, dried over magnesium sulfate, filtered and evaporated to dryness. The crude material is purified by column chromatography (eluent: ethyl acetate). Yield: 182 mg (65%/).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07683076B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-901766c3da9c4015bbc65f2091c113ae |
| Source note | uspto-grants-2010_03 |