反应详情

温度

22.5 °C

To a solution of dimethyl 1-trityl-3,5-pyrazoledicarboxylate (3.200 g, 7.50 mmol) in dry THF (50 mL) were added 30 mL of 1.0 M LiAlH4 in Et2O. The resulting solution was stirred for about 16 h at room temperature (20-25° C.). After this time, the reaction was quenched by the slow addition of 1 mL of distilled water, followed by addition of 1 mL of 10% NaOH and 2.4 mL of water. The solids formed were removed by filtration, and 50 mL of dichloromethane was added to the filtrate. The organic phase was separated, washed with distilled water and a white microcrystalline solid was obtained after evaporation of the solvent under vacuum. Yield: 90% (2.843 g, 6.71 mmol).

1. customAfter this time, the reaction was quenched by the slow addition of 1 mL of distilled water
2. additionfollowed by addition of 1 mL of 10% NaOH and 2.4 mL of water
3. customThe solids formed
4. customwere removed by filtration, and 50 mL of dichloromethane
5. additionwas added to the filtrate
6. customThe organic phase was separated
7. washwashed with distilled water
8. customa white microcrystalline solid was obtained
9. customafter evaporation of the solvent under vacuum