HRID894928

反应详情

EQUATION

反应方程式

HRID 894928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Hydroxybenzoic acid (27.6 g), 4-chloro-3-cyano-benzotrifluoride (41.1 g) and anhydrous potassium carbonate (55.2 g) were stirred together for 71/2 hours at 100° C. in dry dimethylformamide (500 ml) and then left at room temperature for 65 hours. The solvent was then removed under reduced pressure and the residue taken up in water and acidified with dilute hydrochloric acid. The solid which separated was washed with water, dissolved in ether and the solution dried and concentrated. The colourless solid which separated was recrystallised to give the benzoic acid derivative (24.0 g) with a melting point of 224°-226° C.

WORKUP

后处理

  1. customThe solvent was then removed under reduced pressure
  2. customThe solid which separated
  3. washwas washed with water
  4. dissolutiondissolved in ether
  5. customthe solution dried
  6. concentrationconcentrated
  7. customThe colourless solid which separated
  8. customwas recrystallised