HRID2272550

反应详情

EQUATION

反应方程式

HRID 2272550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Bromo-3-methyl-1H-indole (1.33 g) was dissolved in dimethylformamide (20 mL), and sodium hydride (0.33 g) was added thereto under ice-cooling. After stirring at 0° C. for 15 minutes, p-methoxybenzyl chloride (0.95 mL) was added thereto. The reaction solution was stirred under heating at 70° C. for 30 minutes and partitioned between ethyl acetate and 1M HCl aqueous solution. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue was purified by neutral silica gel column chromatography (hexane/ethyl acetate) to obtain compound (45a) (2.09 g, 99%) as a colorless oily substance.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. stirringThe reaction solution was stirred
  3. temperatureunder heating at 70° C. for 30 minutes
  4. custompartitioned between ethyl acetate and 1M HCl aqueous solution
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customAfter removal of the solvent
  8. customby evaporation
  9. customthe residue was purified by neutral silica gel column chromatography (hexane/ethyl acetate)