反应详情

温度

0 °C

Dissolve 3,5-dimethylpyrazole (0.331 g, 3.44 mmol) in N,N-dimethylformamide (7 mL) and add sodium hydride (0.165 g, 4.13 mmol). After 10 min., cool to 0° C. and add 4-methoxybenzyl chloride (0.654 mL, 4.82 mmol) dropwise. Stir the mixture at 25° C. for 18 hr. then dilute with saturated ammonium chloride. Extract with ethyl acetate 3 times, dry (sodium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 40:60 hexanes:ethyl acetate), to give 1-(4-methoxybenzyl)-3,5-dimethyl-1H-pyrazole as a colorless oil (0.682 g, 92%). MS (APCI): m/z=217 [M+H].

1. extractionExtract with ethyl acetate 3 times
2. dry with materialdry (sodium sulfate)
3. filtrationfilter
4. concentrationconcentrate
5. custompurify
6. wash(silica gel chromatography, eluting with 40:60 hexanes:ethyl acetate)