HRID443597

反应详情

EQUATION

反应方程式

HRID 443597 的结构方程式

PROCEDURE

实验过程

174 g of 1-phenyl-3-methyl-pyrazol-5-one in 700 ml of acetic anhydride, with the addition of 6 g of p-toluenesulphonic acid, are heated to the boil under reflux for 6 hours. The solvent is then distilled off under a water-pump vacuum, the residue is dissolved hot in 2 l of 5% strength sodium hydroxide solution, the solution is clarified with 8 g of active charcoal, the filtrate is acidified with hydrochloric acid at room temperature and the crystalline precipitate is filtered off, washed with water and dried in vacuo at 40° C. 183 g of 1-phenyl-3-methyl-4-acetyl-pyrazol-5-one are obtained in the form of colourless crystal needles.

WORKUP

后处理

  1. temperatureare heated to the boil
  2. temperatureunder reflux for 6 hours
  3. distillationThe solvent is then distilled off under a water-pump vacuum
  4. dissolutionthe residue is dissolved hot in 2 l of 5% strength sodium hydroxide solution
  5. customis acidified with hydrochloric acid at room temperature
  6. filtrationthe crystalline precipitate is filtered off
  7. washwashed with water
  8. customdried in vacuo at 40° C