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)101 mg, 0.254 mmol) in DMSO (1 ml) was added cesium carbonate (166 mg, 0.508 mmol) and then 1-bromo-2-(methyloxy)ethane (0.035 ml, 0.372 mmol, Aldrich) under nitrogen at ambient temperature. The solution was stirred for 6 h. The mixture was filtered using a hydrophobic frit and the filtrate diluted with methanol (1 ml). The filtrate was 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 pale yellow gum (35 mg); LCMS: (System 4) MH+=456, tRET=2.84 min.

1. customat ambient temperature
2. filtrationThe mixture was filtered
3. additionthe filtrate diluted with methanol (1 ml)
4. customThe filtrate was purified by MDAP on Sunfire C18 column
5. customThe solvent was evaporated in vacuo