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
19.8 g (0.07 mol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole and 7.1 g (0.09 mol) of pyridine are dissolved in 150 ml of acetonitrile, and 12.1 g (0.09 mol) of tetrahydrofuran-2-carboxylic acid chloride are added at 25°-30° C., with stirring. The mixture is stirred at room temperature for a further 24 hours. The reaction batch is then poured onto water and extracted with chloroform; the chloroform phase is washed with aqueous sodium bicarbonate solution, dried over sodium sulphate and concentrated. The oily residue is crystallized by trituration with petroleum ether. 24 g (87% of theory) of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(2-tetrahydrofuroyl)-amino-pyrazole of melting point 95°-97° C. are obtained.
WORKUP
后处理
- stirringThe mixture is stirred at room temperature for a further 24 hours
- additionThe reaction batch is then poured onto water
- extractionextracted with chloroform
- washthe chloroform phase is washed with aqueous sodium bicarbonate solution
- dry with materialdried over sodium sulphate
- concentrationconcentrated
- customThe oily residue is crystallized by trituration with petroleum ether