反应详情

温度

40 °C

To a solution of dimethyl 4-benzyloxy-1-(2-bromoethyl)-1H-pyrazole-3,5-dicarboxylate (1.0 g, 2.52 mmol) in DMF was added sodium azide. The reaction mixture was stirred at 40° C. overnight and quenched with water (100 mL). The mixture was extracted with EtOAc four times, and the organic extracts were washed with brine, dried over Na2SO4, and concentrated in vacuo. The resulting residue was purified by flash chromatography on silica gel using 0-30% EtOAc/hexanes gradient elution. Collection and concentration of the appropriate fractions afforded the title compound as a white solid. ES MS (M+1)=360.

1. customquenched with water (100 mL)
2. extractionThe mixture was extracted with EtOAc four times
3. washthe organic extracts were washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by flash chromatography on silica gel using 0-30% EtOAc/hexanes gradient elution
7. customCollection and concentration of the appropriate fractions