HRID1983016
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
- 0 °C
PROCEDURE
实验过程
3.50 g of 3-(trifluoromethyl)-1H-pyrazole was suspended in 45 ml of water, and 3.2 g of 50% aqueous solution of sodium hydroxide was added to it. The mixture was cooled to 0° C., and then 3.20 g of bromine was added to the mixture, followed by stirring at room temperature for 7 hours. The reaction mixture was extracted by ethyl acetate. The organic layer was washed with water dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. Hexane was added to the residue, as a result, a crystal was formed. The crystal was collected to obtain 3.38 g of 4-bromo-3-(trifluoromethyl)-1H-pyrazole.
WORKUP
后处理
- extractionThe reaction mixture was extracted by ethyl acetate
- washThe organic layer was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- additionHexane was added to the residue, as a result
- customa crystal was formed
- customThe crystal was collected