反应详情

温度

100 °C

A mixture of 4-nitropyrazole (1000 mg, 8.80 mmol), oxetan-3-ylmethyl methanesulfonate (1.90 g, 11.0 mmol), cesium carbonate (8.70 g, 27.0 mmol) and acetonitrile (13 mL) was heated at 100° C. for 3 h. The mixture was cooled to room temperature, saturated ammonium chloride was added. The mixture was extracted with methylene chloride 3×. Combined organics were dried (Na2SO4) and the solvent removed under reduced pressure. The crude product was purified by flash chromatography eluting with 0 to 70% ethyl acetate in heptane to give 4-nitro-1-(oxetan-3-ylmethyl)pyrazole (1.60 g, 99%).

1. temperatureThe mixture was cooled to room temperature
2. extractionThe mixture was extracted with methylene chloride 3×
3. dry with materialCombined organics were dried (Na2SO4)
4. customthe solvent removed under reduced pressure
5. customThe crude product was purified by flash chromatography
6. washeluting with 0 to 70% ethyl acetate in heptane