HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-chloro-4-[(3'-cyano-3-pyridazin-4-ylbiphenyl-4-yl)oxy]-2-fluoro-N-1,3,4-thiadiazol-2-ylbenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 58042343 | HCID 58042343 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-chloro-4-[(3'-cyano-3-pyridazin-4-ylbiphenyl-4-yl)oxy]-2-fluoro-N-1,3,4-thiadiazol-2-ylbenzenesulfonamide | HCID 56601985 | 70% |
Reaction Steps
5-Chloro-4-(3′-cyano-3-(pyridazin-4-yl)biphenyl-4-yloxy)-N-(2,4-dimethoxybenzyl)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide (Preparation 118, 550 mg, 0.77 mmol) was dissolved in methanol (2 mL) and a 4M solution of hydrogen chloride in 1,4-dioxane (10 mL) was added. The reaction mixture was stirred at room temperature for 18 hours and then concentrated in vacuo. The residue was co-evaporated with methanol and then purified by reverse phase chromatography (acetonitrile/water both with 0.1% formic acid) to give the title compound (303 mg, 70%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772293B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-51e57fb6c2dc4ebabec886d5eca826e3 |
| Source note | uspto-grants-2014_07 |