HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Chloropyridazin-3-ol | HCID 252828 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 2783607 | — |
Reaction Steps
To a solution 6-chloropyridazin-3(2H)-one (130 mg, 1.0 mmol) in acetonitrile (3.0 mL) was added K2CO3 (437 mg, 3.16 mmol), CH3I (299 mg, 2.11 mmol), the reaction mixture was stirred at reflux for 2 h. The mixture was cooled to ambient temperature, diluted with EtOAc (20 mL), washed with sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated. The residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1) to obtained product: LC/MS m/z=145 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273033B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-8a9f4b1f7eea4bc698fd87d0c961aa8d |
| Source note | uspto-grants-2016_03 |