反应 #657259

反应方程式

dimethyl 1-trityl-3,5-pyrazoledicarboxylate

LiAlH4

→

1-trityl-3,5-bis(hydroxymethyl)pyrazole

收率 90.0%

溶剂

THF

Et2O

反应条件

后处理

1. 1
   其他After this time, the reaction was quenched by the slow addition of 1 mL of distilled water
2. 2
   workup.ADDITIONfollowed by addition of 1 mL of 10% NaOH and 2.4 mL of water
3. 3
   其他The solids formed
4. 4
   其他were removed by filtration, and 50 mL of dichloromethane
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   其他The organic phase was separated
7. 7
   洗涤washed with distilled water
8. 8
   其他a white microcrystalline solid was obtained
9. 9
   其他after evaporation of the solvent under vacuum

实验过程

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).

来源