HRID1242143

反应详情

EQUATION

反应方程式

HRID 1242143 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(2,4-Dichlorobenzoyl)-5-(methoxycarbonyl)-2-methylindole (0.60 g) is suspended in ethanol (10 ml), to which is added an aqueous solution of 1.5 M sodium hydroxide (5 ml), and heated under reflux for 3 hours. The reaction mixture is concentrated under reduced pressure, and the residue is made acidic with water and 3 M HCl added thereto. The crystal formed is taken out through filtration, then suspended in ethanol-toluene, and concentrated under reduced pressure for azeotropic dehydration. Next, this is dried on calcium chloride in a vacuum desiccator to obtain a crystal of 5-carboxy-3-(2,4-dichlorobenzoyl)-2-methylindole (76) (0.56 g).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. concentrationThe reaction mixture is concentrated under reduced pressure
  4. additionadded
  5. customThe crystal formed
  6. filtrationis taken out through filtration
  7. concentrationconcentrated under reduced pressure for azeotropic dehydration
  8. customNext, this is dried on calcium chloride in a vacuum desiccator