HRID1848309

反应详情

EQUATION

反应方程式

HRID 1848309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After adding 5.85 g of toluene to 1.95 g (4.81 mmol) of 5-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-fluorobenzonitrile, 1.14 g (9.62 mmol) of thionyl chloride and 0.76 g (9.62 mmol) of pyridine were added at 80° C., and stirred for 2 hours. The reaction solution was cooled to room temperature, and separated by adding 20 ml of toluene and 10 ml of water. After washing the toluene phase with an aqueous solution of 0.39 g of sodium hydroxide dissolved into 10 ml of water, the phase was washed with water. The solvent was distilled off under reduced pressure to obtain 1.59 g of 5-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-2-fluorobenzonitrile (yield 85.2%).

WORKUP

后处理

  1. additionwere added at 80° C.
  2. customseparated
  3. additionby adding 20 ml of toluene and 10 ml of water
  4. washAfter washing the toluene phase with an aqueous solution of 0.39 g of sodium hydroxide
  5. dissolutiondissolved into 10 ml of water
  6. washthe phase was washed with water
  7. distillationThe solvent was distilled off under reduced pressure