HRID1489147

反应详情

EQUATION

反应方程式

HRID 1489147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A 90 g portion of the abovementioned methyl (3-methoxystyryl) ether was dissolved in 100 ml of ethanol. Then the solution was added dropwise to a mixed solution of 59.3 g phenylhydrazine, 800 ml ethanol and 53 ml concentrated hydrochloric acid under reflux, and after the addition, reflux heating was continued for 2 more hours. The reaction mixture was then cooled to room temperature, and after adding water, sodium chloride and a small amount of ethyl acetate, the mixture was stirred and the precipitated crystals were collected by filtration. The crystals were dissolved in chloroform and washed with dilute hydrochloric acid and sodium bicarbonate aqueous solution. And the solution was dried and concentrated to obtain a residue. Then toluene was added to the residue, and after refluxed for one hour. After cooling, precipitated crystals were then collected by filtration to obtain 89.6 g of 3-(3-methoxyphenyl)indole.

WORKUP

后处理

  1. temperatureunder reflux
  2. additionafter the addition
  3. temperaturereflux
  4. temperatureheating
  5. filtrationthe precipitated crystals were collected by filtration
  6. dissolutionThe crystals were dissolved in chloroform
  7. washwashed with dilute hydrochloric acid and sodium bicarbonate aqueous solution
  8. customAnd the solution was dried
  9. concentrationconcentrated
  10. customto obtain a residue
  11. temperatureafter refluxed for one hour
  12. temperatureAfter cooling
  13. customprecipitated crystals
  14. filtrationwere then collected by filtration