تفاعل #342007

معادلة التفاعل

5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile

sodium azide

ammonium chloride

→

5-(5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazol-3-yl)-1H-tetrazole

المردود 98.0%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىwas placed in a microwave synthesizer tube
2. 2
   أخرىirradiation in a Biotage® Initiator
3. 3
   أخرىwas set at 180° C
4. 4
   أخرىthe mixture was quenched with water
5. 5
   استخلاصextracted with ethyl acetate
6. 6
   أخرىThe solvent of the extracted organic layer was evaporated off
7. 7
   أخرىthe residue was purified by reverse phase preparative HPLC

الإجراء التجريبي

A mixture of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile (500 mg, 1.39 mmol), sodium azide (1.08 g, 16.6 mmol) and ammonium chloride (890 mg, 16.6 mmol) dissolved in dimethylformamide (3 ml) was placed in a microwave synthesizer tube, and subjected to microwave irradiation in a Biotage® Initiator was set at 180° C. After 20 minutes, the mixture was quenched with water and extracted with ethyl acetate. The solvent of the extracted organic layer was evaporated off and the residue was purified by reverse phase preparative HPLC, to obtain 5-(5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazol-3-yl)-1H-tetrazole (550 mg, 98%) as white solid.

المصدر