HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58128682, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 58128717 | HCID 58128717 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58128682 | HCID 58128682 | 51.5% |
Reaction Steps
To a solution of 4-[3-(2,5-dimethyl-pyrrol-1-yl)-4-methyl-phenyl]-2-methyl-2H-pyridazin-3-one (1.05 g, 3.57 mmol) in EtOH (20 ml) and water (10 ml) was added hydroxyl amine hydrochloride (2.49 g, 35.79 mmol) and triethyl amine (1.0 ml, 7.16 mmol). The mixture was heated at reflux for 24 hours. The solvent was evaporated to dryness under reduced pressure and the rsidue was partitioned between water and EtOAc. The organic layer was separated and washed with water and brine, dried over MgSO4, filtered and concentrated to dryness under reduced pressure. Purification of the residue by flash chromatography (hex:EtOAc/1:1) gave 0.396 g (51%) of 4-(3-amino-4-methyl-phenyl)-2-methyl-2H-pyridazin-3-one as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08435990B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-f913e801d4644ac884dbdb78965ef90d |
| Source note | uspto-grants-2013_05 |