反应详情

To a solution of 2,6-difluoro-N-{1-[(5-hydroxy-2-methylphenyl)methyl]-1H-pyrazol-3-yl}benzamide (for a preparation see Intermediate 49)(82 mg, 0.239 mmol) in DMSO (1 ml) was added cesium carbonate (155 mg, 0.476 mmol) and then a solution of 1-bromo-3-(methyloxy)propane (45 mg, 0.294 mmol, Matrix Scientific) in DMSO (0.1 ml). The resulting red solution was stirred at ambient temperature under nitrogen overnight. The solution was filtered using a hydrophobic frit and diluted with methanol (0.9 ml). The mixture was purified by MDAP on a Sunfire C18 column (Method B) using Acetonitrile-Water with a Formic acid modifier. The solvent was evaporated in vacuo to give the title compound as a luminous yellow gum (19.4 mg); LCMS (System 4) MH+=416, tRET=2.79 min.

1. filtrationThe solution was filtered
2. additiondiluted with methanol (0.9 ml)
3. customThe mixture was purified by MDAP on a Sunfire C18 column (Method B)
4. customThe solvent was evaporated in vacuo