HRID750111

反应详情

EQUATION

反应方程式

HRID 750111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-chlorophthalic anhydride (25 g) in benzene (200 ml) was added aluminum chloride (36.5 g), and the mixture was stirred at room temperature for 1 hr. and subsequently refluxed for 30 min. After cooling the reaction mixture, it was diluted with ethyl acetate (200 ml) and poured into ice water. Conc. hydrochloric acid (20 ml) was added and the mixture was stirred at room temperature for 30 min. After separating the organic layer, the layer was washed successively with 4N hydrochloric acid, water and brine, dried over sodium sulfate and concentrated until the crystals precipitated. The crystals were collected by filtration and washed with isopropyl ether to give 4-chloro-2-benzoylbenzoic acid (16 g) as colorless crystals.

WORKUP

后处理

  1. temperatureand subsequently refluxed for 30 min
  2. temperatureAfter cooling the reaction mixture, it
  3. stirringthe mixture was stirred at room temperature for 30 min
  4. customAfter separating the organic layer
  5. washthe layer was washed successively with 4N hydrochloric acid, water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated until the crystals
  8. customprecipitated
  9. filtrationThe crystals were collected by filtration
  10. washwashed with isopropyl ether