HRID743054

反应详情

EQUATION

反应方程式

HRID 743054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 23.2 g (100 mmol) of 2-amino-5-chlorobenzophenone and 11 g (110 mmol) of triethylamine in 200 mL of tetrahydrofuran was added dropwise 20 g (110 mmol) of trichloroacetyl chloride at temperature of 5° C. to 15° C. After being stirred for 3 hours at ambient temperature, the reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The organic layer separated was washed with water and then with brine, dried on anhydrous sodium sulfate and concentrated in vacuo. The resulting crude crystals were recrystallized from ethanol to give 33.8 g (89.9 mmol) of the title compound.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe organic layer separated
  3. washwas washed with water
  4. dry with materialwith brine, dried on anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting crude crystals were recrystallized from ethanol