تفاعل #657261

معادلة التفاعل

trimethyl 1-trityl-3,4,5-pyrazoletricarboxylate

LiAlH4

→

1-trityl-3,4,5-tris(hydroxymethyl)pyrazole

المردود 73.0%

المذيبات

THF

Et2O

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter this time, the reaction was quenched by the slow addition of 1.5 mL of distilled water
2. 2
   workup.ADDITIONfollowed by addition of 1.5 mL of 10% NaOH and 3.5 mL of water
3. 3
   أخرىThe solids formed
4. 4
   أخرىwere removed by filtration, and 80 mL of dichloromethane
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   أخرىThe organic phase was separated
7. 7
   غسيلwashed with distilled water (70 mL)
8. 8
   أخرىafter separation from the aqueous phase
9. 9
   تجفيفwas dried over MgSO4
10. 10
    أخرىAfter separation of the organic phase
11. 11
    أخرىthe solvent was evaporated under vacuum
12. 12
    أخرىyielding a yellowish solid

الإجراء التجريبي

To a solution of trimethyl 1-trityl-3,4,5-pyrazoletricarboxylate (3.034 g, 6.26 mmol) in dry THF (60 mL) were added 50 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 1.5 mL of distilled water, followed by addition of 1.5 mL of 10% NaOH and 3.5 mL of water. The solids formed were removed by filtration, and 80 mL of dichloromethane was added to the filtrate. The organic phase was separated, washed with distilled water (70 mL) and, after separation from the aqueous phase, was dried over MgSO4. After separation of the organic phase, the solvent was evaporated under vacuum yielding a yellowish solid. Yield: 73% (1.823 g, 4.54 mmol).

المصدر