HRID1708854

反应详情

EQUATION

反应方程式

HRID 1708854 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

Next, 57 g (0.15 mol) of the 1-(2,4,6-trichlorophenyl)-3-acetylamino-4-bromo-5-oxo-2-pyrazoline and 41 g of pyrazole (0.6 mol) were mixed well, then heated for 6 hours at 75° C. in a stream of nitrogen gas to react, after which the reaction mixture was cooled to room temperature. Next the reaction mixture was dissolved in ethyl acetate and the solution was washed with water three times and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, acetonitrile was added to the residual oil, and the deposited crystals were filtered to obtain 20.1 g (34.7%) of 1-(2,4,6-trichlorophenyl)-3-acetylamino-4-pyrazolyl-5-oxo-2pyrazoline.

WORKUP

后处理

  1. customto react
  2. temperatureafter which the reaction mixture was cooled to room temperature
  3. washthe solution was washed with water three times
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure, acetonitrile
  6. additionwas added to the residual oil
  7. filtrationthe deposited crystals were filtered