HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 59547883, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 59547885 | HCID 59547885 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 59547883 | HCID 59547883 | 14.9% |
Reaction Steps
To a solution of N-{1-[(2-chloro-5-hydroxyphenyl)methyl]-1H-pyrazol-3-yl}-2,6-difluorobenzamide (for as preparation see Intermediate 13) (73 mg, 0.20 mmol) in DMSO (0.5 ml) was added potassium t-butoxide (21 mg, 0.187 mmol). The reaction was stirred for 5 min before adding methyl iodide (0.012 mL, 0.201 mmol, Aldrich). The reaction was stirred at ambient temperature, overnight and under nitrogen. The reaction mixture was filtered through a hydrophobic frit and the filtrate diluted with methanol (0.5 ml) and the sample purified by MDAP on Sunfire C18 column using Acetonitrile-Water with a Formic acid modifier (Method B). The solvent was evaporated in vacuo to give the title compound (10.5 mg); LCMS: (System 4) MH+=378, tRET=2.86 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399436B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-e396760adf7e48ef97d304f195ccd447 |
| Source note | uspto-grants-2013_03 |