반응 #1583841

반응 방정식

cesium carbonate

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

salicylaldoxime

5-bromo-2-chlorotoluene

→

title compound

수율 21.7%

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

수율 21.7%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타prepared
2. 2
   온도to cool to room temperature
3. 3
   여과The resulting suspension was filtered
4. 4
   농축the filtrate was concentrated
5. 5
   기타The resulting residue was purified by medium pressure liquid chromatography (2 to 10% gradient of ethyl acetate in hexanes as eluant)

실험 절차

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).

출처