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)(100 mg, 0.252 mmol) in DMSO (1 ml) was added cesium carbonate (166 mg, 0.509 mmol) and then 3-(bromomethyl)pyridine hydrobromide (89 mg, 0.352 mmol, Aldrich) at ambient temperature under nitrogen. The resulting yellow suspension was stirred for 3 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 TFA modifier (Method C). The solvent was evaporated in vacuo to give the title compound (65 mg) as a yellow solid; LCMS: (System 4) MH+=489, tRET=2.25 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