反应 #156291

反应方程式

1-(4-bromo-2-nitrophenyl)butane-1,3-dione

cyclopentylhydrazine hydrochloride

→

5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-3-methyl-1H-pyrazole

收率 62.9%

溶剂

acetic acid

反应条件

后处理

1. 1
   浓缩The reaction mixture was concentrated
2. 2
   workup.ADDITIONto the obtained residue was added ethyl acetate
3. 3
   洗涤The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   其他The solvent was evaporated under reduced pressure
6. 6
   其他the residue was purified by silica gel column chromatography (chloroform/methanol)

实验过程

Under a nitrogen atmosphere, to a solution of 1.0 g of 1-(4-bromo-2-nitrophenyl)butane-1,3-dione in 10 ml of acetic acid was added 501 mg of cyclopentylhydrazine hydrochloride, followed by stirring at 100° C. for 1 hour and 30 minutes. The reaction mixture was concentrated, and to the obtained residue was added ethyl acetate. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and then the residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 770 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-3-methyl-1H-pyrazole.

来源