HRID2187751

反应详情

EQUATION

反应方程式

HRID 2187751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-(Methoxycarbonyl)-3-methylindole (0.57 g) is dissolved in N,N-dimethylformamide (10 ml), to which is added sodium hydride (60% oily, 0.145 g) with cooling with ice. Then, 2,4-dichlorobenzyl chloride (0.707 g) is added thereto, and stirred at room temperature for 1.5 hours. Water is added to the reaction mixture, which is then extracted with ethyl acetate. The organic layer is washed with a saturated saline solution, and dried with anhydrous magnesium sulfate. The drying agent is removed through filtration, and the filtrate is concentrated under reduced pressure. The resulting residue is purified through silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to obtain 1-(2,4-dichlorobenzyl)-6-(methoxycarbonyl)-3-methylindole (72) (0.83 g).

WORKUP

后处理

  1. temperaturewith cooling with ice
  2. extractionis then extracted with ethyl acetate
  3. washThe organic layer is washed with a saturated saline solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe drying agent is removed through filtration
  6. concentrationthe filtrate is concentrated under reduced pressure
  7. customThe resulting residue is purified through silica gel column chromatography (eluent: hexane/ethyl acetate=9/1)