HRID2290714

反应详情

EQUATION

反应方程式

HRID 2290714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

33.4 g of 3,5-dichloro-4-(1,1,2,2,-tetrafluoroethoxy)aniline are dissolved in 130 ml of chlorobenzene. With stirring, this solution is added dropwise at 22° C. to a solution consisting of 90 g of toluene containing 20% by weight of phosgene and of 100 ml of dioxane and 300 ml of chlorobenzene. The reaction mixture is stirred for 1 hour at room temperature, 1 hour at 50° C. and then 1 hour at 80° C. The reaction mixture is subsequently concentrated in a water-jet vacuum and then distilled under high vacuum, affording the title compound of the formula ##STR8## as a colourless oil. Boiling point 81°-83° C./2.5 mbar.

WORKUP

后处理

  1. additionthis solution is added dropwise at 22° C. to a solution
  2. stirringThe reaction mixture is stirred for 1 hour at room temperature, 1 hour at 50° C.
  3. custom1 hour
  4. customat 80° C
  5. concentrationThe reaction mixture is subsequently concentrated in a water-jet vacuum
  6. distillationdistilled under high vacuum