تفاعل #657259

معادلة التفاعل

dimethyl 1-trityl-3,5-pyrazoledicarboxylate

LiAlH4

→

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

المردود 90.0%

المذيبات

THF

Et2O

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter 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
   أخرىThe solids formed
4. 4
   أخرىwere removed by filtration, and 50 mL of dichloromethane
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   أخرىThe organic phase was separated
7. 7
   غسيلwashed with distilled water
8. 8
   أخرىa white microcrystalline solid was obtained
9. 9
   أخرىafter evaporation of the solvent under vacuum

الإجراء التجريبي

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).

المصدر