HRID2309401

反应详情

EQUATION

反应方程式

HRID 2309401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.1 g of 2,6-dimethyl-4-propionylphenol and 5.0 g of 4-methoxyphenylhydrazine hydrochloride were dispersed in 30 ml of isopropanol, and the dispersion was refluxed for 20 hours in a nitrogen stream. Water was added to the reaction mixture, and the precipitated crystals were collected by filtration. The crystals were dissolved in ethyl acetate, and washed with a 5% aqueous sodium hydroxide solution, water, 2N hydrochloric acid and water. The organic layer was dried, and the solvent was evaporated. Recrystallization of the resulting crude crystals from ethanol-hexane gave 5.8 g of 2-(4-hydroxy-3,5-dimethylphenyl)-5-methoxy-3-methylindole.

WORKUP

后处理

  1. temperaturethe dispersion was refluxed for 20 hours in a nitrogen stream
  2. filtrationthe precipitated crystals were collected by filtration
  3. dissolutionThe crystals were dissolved in ethyl acetate
  4. washwashed with a 5% aqueous sodium hydroxide solution, water, 2N hydrochloric acid and water
  5. customThe organic layer was dried
  6. customthe solvent was evaporated
  7. customRecrystallization of the resulting crude crystals from ethanol-hexane