HRID1863350

反应详情

EQUATION

反应方程式

HRID 1863350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Aluminum trichloride (11.75 g.; 0.088 mole) was added portionwise to a stirred mixture of the p-chlorophenylacetyl chloride and chlorobenzene (30 ml.). Following addition, the mixture was allowed to stand for 24 hours. The resulting dark brown paste was scooped out and stirred into a slurry of ice and conc. hydrochloric acid which was then extracted with methylene chloride. The organic extracts were washed with 1 N hydrochloric acid, saturated sodium bicarbonate, saturated sodium chloride; dried over sodium sulfate and concentrated in vacuo. Recrystallization from methanol afforded 16.47 g. (71% yield), m.p. 111.5°-114° C.

WORKUP

后处理

  1. additionaddition
  2. extractionwas then extracted with methylene chloride
  3. washThe organic extracts were washed with 1 N hydrochloric acid, saturated sodium bicarbonate, saturated sodium chloride
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customRecrystallization from methanol
  7. customafforded 16.47 g