تفاعل #1583841

معادلة التفاعل

cesium carbonate

3-(3-chlorophenyl)-1H-pyrazole

salicylaldoxime

5-bromo-2-chlorotoluene

→

title compound

المردود 21.7%

1-(3-methyl-4-chlorophenyl)-3-(3-chlorophenyl)-1H-pyrazole

المردود 21.7%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared
2. 2
   درجة الحرارةto cool to room temperature
3. 3
   ترشيحThe resulting suspension was filtered
4. 4
   تركيزthe filtrate was concentrated
5. 5
   أخرىThe resulting residue was purified by medium pressure liquid chromatography (2 to 10% gradient of ethyl acetate in hexanes as eluant)

الإجراء التجريبي

A mixture of 3-(3-chlorophenyl)-1H-pyrazole (5.3 g, 29.8 mmol) (prepared according to the method given in European Patent Publication EP 538156), salicylaldoxime (0.58 g, 4.25 mmol), 5-bromo-2-chlorotoluene (2.8 g, 21.3 mmol), copper oxide (0.15 g, 1.06 mmol) and cesium carbonate (11.8 g, 36.2 mmol) in 20 mL of N,N-dimethylformamide was heated at 140° C. overnight and then allowed to cool to room temperature. The resulting suspension was filtered and the filtrate was concentrated under reduce pressure. The resulting residue was purified by medium pressure liquid chromatography (2 to 10% gradient of ethyl acetate in hexanes as eluant) to give the title compound as a white solid (1.4 g).

المصدر