HRID622594

反应详情

EQUATION

反应方程式

HRID 622594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe mixture is stirred at room temperature for a further 24 hours
  2. additionThe reaction batch is then poured onto water
  3. extractionextracted with chloroform
  4. washthe chloroform phase is washed with aqueous sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. customThe oily residue is crystallized by trituration with petroleum ether