HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4,6-Trichloropyridazine → 3,6-Dichloro-4-methanesulfonylpyridazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4,6-Trichloropyridazine | HCID 95123 | — |
| Reactant | Sodium methanesulfinate | HCID 2733271 | — |
| Solvent | water THF DMF | HCID 86606902 | — |
| Product | 3,6-Dichloro-4-methanesulfonylpyridazine | HCID 58045789 | — |
Reaction Steps
3,4,6-Trichloropyridazine (2.5 g; 13.6 mmol) and methanesulfinic acid sodium salt (2.78 g, 27.26 mmol) were stirred in 20 ml of a solvent mixture of water/THF/DMF (5:10:5) at RT for 30 h. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and saturated ammonium chloride solution. The organic phase was removed and concentrated, and the crude product was purified by flash chromatography (dichloromethane:methanol). Yield: 1.4 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09079906B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-2a4c6fcd11624d588d842a8da755c32f |
| Source note | uspto-grants-2015_07 |