HRID868464

反应详情

EQUATION

反应方程式

HRID 868464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3-Hydroxybenzoic acid (3.45 g) was added to a solution of potassium hydroxide (2.8 g) in methanol. The solution was evaporated under reduced pressure to give a white solid. This was taken up in dry dimethylsulphoxide (25 ml). The resulting solution was stirred and heated at 170° with anhydrous potassium carbonate (1.25 g) and 4-chloro-3-fluorobenzotrifluoride (5 g) for 12 hours. The mixture was then cooled and poured into water, (500 ml). The mixture was extracted with ether and then acidified (HCl). The precipitate which formed was recrystallised from petroleum (b.p. 60°-80°) to give the required acid (4.5 g) with a melting point of 142°-143°.

WORKUP

后处理

  1. customThe solution was evaporated under reduced pressure
  2. customto give a white solid
  3. temperatureThe mixture was then cooled
  4. extractionThe mixture was extracted with ether
  5. customThe precipitate which formed
  6. customwas recrystallised from petroleum (b.p. 60°-80°)