反应详情

温度

80 °C

To a stirred solution of potassium 2-(4-(1H-pyrazol-1-yl)phenyl)-2-methoxyacetate (˜7.55 mmol) in dry MeOH under argon was added sulfuric acid (2.0 mL) dropwise. The mixture was heated at 80° C. for 17 hours. After cooling to room temperature, water was added then the mixture made basic with saturated aqueous NaHCO3 addition. The aqueous phase was extracted with EtOAc and the combined organics were washed with water and brine then dried over Na2SO4 and concentrated in vacuo. Purification by chromatography (20-35% EtOAc-hexanes) provided methyl 2-(4-(1H-pyrazol-1-yl)phenyl)-2-methoxyacetate as a colorless oil (0.88 g, 47% yield for two steps).

1. temperatureAfter cooling to room temperature
2. extractionThe aqueous phase was extracted with EtOAc
3. washthe combined organics were washed with water and brine
4. dry with materialthen dried over Na2SO4
5. concentrationconcentrated in vacuo
6. customPurification by chromatography (20-35% EtOAc-hexanes)