反应详情

NaH (0.594 g, 14.84 mmol) was suspended in THF (10 mL), and 3,5-dimethylpyrazole (1.091 g, 11.35 mmol) was slowly added and stirred for one hour at room temperature. 2-Chloropyrimidine (1 g, 8.73 mmol) was slowly added to the mixture and refluxed for three hours. Completion of the reaction was confirmed by TLC, and then water (5 mL) was added to the mixture. The solvent was distilled off and the residue was extracted with ethyl acetate twice. The organic phase was washed with saturated brine and dried over magnesium sulfate. The solvent was then distilled off and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2→ethyl acetate) to give 1.05 g of the title compound (yield 69%).

1. temperaturerefluxed for three hours
2. distillationThe solvent was distilled off
3. extractionthe residue was extracted with ethyl acetate twice
4. washThe organic phase was washed with saturated brine
5. dry with materialdried over magnesium sulfate
6. distillationThe solvent was then distilled off
7. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2→ethyl acetate)