反应详情

To a solution of 2,6-difluoro-N-(1-{[4-hydroxy-2-(trifluoromethyl)phenyl]methyl}-1H-pyrazol-3-yl)benzamide (for a preparation see Example 36)(72 mg, 0.181 mmol) in DMSO (0.5 ml) was added potassium t-butoxide (20 mg, 0.178 mmol). The reaction mixture was stirred for 5 min before adding methyl iodide (0.011 ml, 0.181 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 as a white solid (20.3 mg);

1. stirringThe reaction was stirred at ambient temperature, overnight and under nitrogen
2. filtrationThe reaction mixture was filtered through a hydrophobic frit
3. additionthe filtrate diluted with methanol (0.5 ml)
4. customthe sample purified by MDAP on Sunfire C18 column
5. customThe solvent was evaporated in vacuo