反应详情

温度

130 °C

To a stirred solution of 1-{[3-(4-fluorophenyl)-1H-pyrazol-5-yl]oxy}acetone (0.25 g, 1.0 mmol) in toluene, equipped with dean stark apparatus, acetic acid (2 ml) and p-TsOH (25 mg, cat.) was charged at RT and the reaction mass was refluxed at 130° C. for 16 h. After completion, the reaction was diluted with EtOAc (50 ml) and washed with brine. The organic layer dried over sodium sulphate and concentrated under reduced pressure to get the crude which was then purified by column chromatography 100-200 mesh) eluted with 5-10% ethyl acetate in hexane as eluent to get compound 6-(4-fluorophenyl)-3-methylpyrazolo[5,1-b][1,3]oxazole (0.1 g, yield 43%).

1. additionwas charged at RT
2. washwashed with brine
3. dry with materialThe organic layer dried over sodium sulphate
4. concentrationconcentrated under reduced pressure
5. customto get the crude which
6. customwas then purified by column chromatography 100-200 mesh)
7. washeluted with 5-10% ethyl acetate in hexane as eluent