反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of 5-bromo-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoromethylsulfonylpyrazole (2.5 g, 4.8 mmol) in 1,4-dioxane and N,N-dimethylformamide was added 2-methoxyethylamine (0.74 g, 9.7 mmol) and potassium carbonate (1.35 g, 9.7 mmol). The resulting mixture was stirred at 50° C. for 4 hours, left to stand overnight, then poured into a mixture of water and dichloromethane. The organic phase was washed with water, dried (sodium sulfate), evaporated. The crude product was recrystallised from diisopropylether to give 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-(2-methoxyethylamino)4-trifluoromethylsulfonylpyrazole as a white solid (Compound number 1-3, 1.30 g), mp 164° C.
WORKUP
后处理
- waitleft
- waitto stand overnight
- washThe organic phase was washed with water
- dry with materialdried (sodium sulfate)
- customevaporated
- customThe crude product was recrystallised from diisopropylether