反应详情

Diphenylphosphoryl azide (2.16 mL) was added to a mixture of 4-benzyloxy-1-(2-fluorophenyl)pyrazole-3-carboxylic acid (2.09 g) and triethylamine (1.39 mL) in a mixture of 1,4-dioxane (25 mL) and tBuOH (25 mL). The mixture was refluxed for 1 hour and cooled to room temperature. The mixture was diluted with EtOAc and washed with H2O, 10% aq. citric acid, sat. NaHCO3 and brine. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (EtOAc/hexane 1/19, 1/9, 1/4 and 1/2) to yield 1.30 g of the title compound.

1. temperatureThe mixture was refluxed for 1 hour
2. washwashed with H2O, 10% aq. citric acid, sat. NaHCO3 and brine
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash chromatography on silica gel (EtOAc/hexane 1/19, 1/9, 1/4 and 1/2)