HRID337327

反应详情

EQUATION

反应方程式

HRID 337327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.50 g of 2-methoxyphenyl hydrazine hydrochloride was dissolved in 60 ml of ethanol, and 2.06 ml of acetyl acetone was added and heated at reflux for 1 hour. To the reaction mixture was added 150 ml of water, neutralized with saturated aqueous solution of sodium carbonate, and extracted with 150 ml of ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure and purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to yield 3.88 g of the title compound.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. extractionextracted with 150 ml of ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. custompurified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)