HRID230082
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
PROCEDURE
实验过程
3.0 g of 3-(2,6-difluorophenyl)pyrazole was dissolved in 20 ml of acetonitrile, and 2.52 g of chloroacetonitrile and 4.61 g of potassium carbonate were added thereto at room temperature, and heated under reflux for 5 hours. After acetonitrile was distilled off under reduced pressure, ethyl acetate was added to the residue, which was then washed with a small amount of water. The organic layer was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether to obtain 1.74 g of 1-cyanomethyl-3-(2,6-difluorophenyl)pyrazole.
WORKUP
后处理
- temperatureunder reflux for 5 hours
- distillationAfter acetonitrile was distilled off under reduced pressure, ethyl acetate
- additionwas added to the residue, which
- washwas then washed with a small amount of water
- dry with materialThe organic layer was dried over sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether