HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 54578953, compound → HCID 178448623, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 54578953 | HCID 54578953 | — |
| Reactant | HCID 67994474 | HCID 67994474 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178448623 | HCID 178448623 | 38.9% |
Reaction Steps
A mixture of 4-(butylamino)-5-chloro-2-methylpyridazin-3(2H)-one from Example 4A (130 mg, 0.60 mmol) and 2-fluoro-5-(trifluoromethyl)benzoyl isothiocyanate (248 mg, 1 mmol) in dioxane (20 mL) was heated at reflux for 72 hours. The mixture was concentrated under reduced pressure and the residue was dissolved in EtOAc, washed with saturated aqueous NaHCO3 and brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by chromatography (hexanes-EtOAc 3:1) to afford 100 mg of the title compound. MS (ESI) m/z 215 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08586596B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-ab4b1655037a43908d9d567bf9ce85dc |
| Source note | uspto-grants-2013_11 |