反应详情

To a mixture of 4-bromo-5-(2,6-difluoro-3-nitrophenyl)-1H-pyrazole (0.88 g, 2.9 mmol) and methyl iodide (2 mL, 32 mmol) in dichloromethane (20 mL), tetrabutylammonium bromide (0.32 g, 1 mmol) in 7 N sodium hydroxide (20 mL) was added and the mixture was rapidly stirred at room temperature for 3 h. The phases were separated and the organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated. The crude residue was purified by flash chromatography (eluant: dichloromethane/petroleum ether 2:1). The title compound, mixture of the two regioisomers, was obtained as a waxy solid (0.53 g, 57%).

1. additionwas added
2. customThe phases were separated
3. washthe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe crude residue was purified by flash chromatography (eluant: dichloromethane/petroleum ether 2:1)
7. additionThe title compound, mixture of the two regioisomers