反応 #657259

反応方程式

dimethyl 1-trityl-3,5-pyrazoledicarboxylate

LiAlH4

→

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

収率 90.0%

溶媒

THF

Et2O

反応条件

後処理

1. 1
   その他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
   その他The solids formed
4. 4
   その他were removed by filtration, and 50 mL of dichloromethane
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   その他The organic phase was separated
7. 7
   洗浄washed with distilled water
8. 8
   その他a white microcrystalline solid was obtained
9. 9
   その他after evaporation of the solvent under vacuum

実験手順

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).

出典