HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-Bromo-6-chloro-2,3-dihydropyridazin-3-one | HCID 11586522 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 59216474 | 97.5% |
Reaction Steps
4-Bromo-6-chloro-2H-pyridazin-3-one (5.02 g, 23.97 mmol) was dissolved in 40 ml dimethylformamide. Cesium carbonate (9.37 g, 28.76 mmol) was added. After 5 min, iodomethane (5.103 g, 35.95 mmol) was added dropwise over 20 min. The reaction mixture was stirred 3 hours at room temperature. The precipitate was filtered off and concentrated and the resulting residue was treated with 20 ml dichloromethane. The insoluble material was filtered off again and washed with dichloromethane. The filtrate was concentrated in vacuo to yield 4-Bromo-6-chloro-2-methyl-2H-pyridazine-3-one (5.223 g, 23.37 mmol). MS (ESI) 224.9 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822457B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-4716460160e64d4f9fd22f14877dfffc |
| Source note | uspto-grants-2014_09 |