反应 #1583841

反应方程式

cesium carbonate

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

salicylaldoxime

5-bromo-2-chlorotoluene

→

title compound

收率 21.7%

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

收率 21.7%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他prepared
2. 2
   温度to cool to room temperature
3. 3
   过滤The resulting suspension was filtered
4. 4
   浓缩the filtrate was concentrated
5. 5
   其他The resulting residue was purified by medium pressure liquid chromatography (2 to 10% gradient of ethyl acetate in hexanes as eluant)

实验过程

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).

来源