反应详情

温度

60 °C

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)(81 mg, 0.204 mmol) in DMSO (0.5 ml) was added potassium t-butoxide (23 mg, 0.205 mmol). The reaction was stirred for 15 min before adding methyl bromoacetate (0.020 ml, 0.211 mmol, Aldrich). The reaction was heated to 60° C. and stirred overnight, 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 brown gum (38.5 mg); LCMS: (System 4) MH+=470, tRET=2.90 min.

1. stirringstirred overnight, 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