HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-Chloro-2-fluoro-4-{[3-pyridazin-4-yl-4'-(trifluoromethyl)biphenyl-4-yl]oxy}-N-pyrimidin-2-ylbenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5-Chloro-N-(2,4-dimethoxybenzyl)-2-fluoro-4-{[3-pyridazin-4-yl-4'-(trifluoromethyl)biphenyl-4-yl]oxy}-N-pyrimidin-2-ylbenzenesulfonamide | HCID 58042347 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-Chloro-2-fluoro-4-{[3-pyridazin-4-yl-4'-(trifluoromethyl)biphenyl-4-yl]oxy}-N-pyrimidin-2-ylbenzenesulfonamide | HCID 56600580 | 42.4% |
Reaction Steps
5-Chloro-N-(2,4-dimethoxybenzyl)-2-fluoro-4-{[3-pyridazin-4-yl-4′-(trifluoromethyl)biphenyl-4-yl]oxy}-N-pyrimidin-2-ylbenzenesulfonamide (Preparation 48) 356 mg, 0.47 mmol) was dissolved in 1,4-dioxane (1.5 mL) and a 4M solution of hydrogen chloride in 1,4-dioxane (2.4 mL) added. The mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated in vacuo and the resulting residue purified by reverse phase preparative HPLC (Trilution method) to afford the title compound as a white solid (120 mg, 42%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772293B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-62e5b22bafce42668224b7bb4ebd4aa4 |
| Source note | uspto-grants-2014_07 |