反应详情

In a round bottom flask was placed 2-methyl-1-(3-nitro-pyrazol-1-yl)-propan-2-ol (1.39 g, 7.51 mmol) dissolved in N,N-dimethylformamide (25 mL). To this solution was added sodium hydride (667 mg, 9.01 mmol, 60% dispersion in oil) and it was stirred for 15 min until gas evolution ceased. To this was then added methyl iodide (700 μL, 11.26 mmol) and it was stirred for 2 h at 25° C. The reaction was then quenched with water (250 mL). The reaction was transferred to a separatory funnel and extracted with ethyl acetate (250 mL). The organics were dried over sodium sulfate and then concentrated with silica gel (3 g) in vacuo and purified on Biotage Flash chromatography system (40M column, silica gel, 20% ethyl acetate/hexanes) to afford 1-(2-methoxy-2-methyl-propyl)-3-nitro-1H-pyrazole (1.33 g, 88%) as a colorless oil.

1. customIn a round bottom flask was placed
2. customThe reaction was then quenched with water (250 mL)
3. customThe reaction was transferred to a separatory funnel
4. extractionextracted with ethyl acetate (250 mL)
5. dry with materialThe organics were dried over sodium sulfate
6. concentrationconcentrated with silica gel (3 g) in vacuo
7. custompurified on Biotage Flash chromatography system (40M column, silica gel, 20% ethyl acetate/hexanes)