HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68014660, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 68014668 | HCID 68014668 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68014660 | HCID 68014660 | 97.5% |
Reaction Steps
A suspension of 1-[4-(3,4-difluoro-1H-pyrrol-1-yl)-2-hydroxyphenyl]-5-methoxy-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4(1H)-one (231 mg), iodomethane (0.0375 mL) and potassium carbonate (138 mg) in DMF (2.5 mL) was stirred at room temperature overnight. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (NH, THF), and recrystallized from methanol/water to give the title compound (232 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09090586B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-f1e0d179e75d48d595403227a3002b6d |
| Source note | uspto-grants-2015_07 |