HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Methoxide → HCID 89876399, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 68497664 | HCID 68497664 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89876399 | HCID 89876399 | 65.3% |
Reaction Steps
6-bromo-4,5-dichloro-2-methyl-pyridazin-3-one (1.5 g, 5.8 mmol) is dissolved in 1,4-dioxane (150 ml). Sodium methoxide (1.5 ml, 25 mass % methanolic solution, 6.4 mmol) is added dropwise and the reaction stirred for 2 h. The mixture is concentrated to a volume of 50 ml then diluted with 50 ml EtOAc. It is washed with 2×35 ml aqueous saturated brine. The organic layer is dried thoroughly over sodium sulfate, filtered and concentrated in vacuo. The crude residue so obtained was purified by flash chromatography (silica gel, eluant a 0-10% EtOAc in Isohexane gradient) to afford 6-bromo-5-chloro-4-methoxy-2-methyl-pyridazin-3-one (960 mg) as a white solid (65% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09049864B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-d42dd5719e104bbd85e75cce02e462d1 |
| Source note | uspto-grants-2015_06 |