HRID133170

反应详情

EQUATION

反应方程式

HRID 133170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
57.5 °C

PROCEDURE

实验过程

104.8 g of 1-(4-methylphenyl)hydrazine hydrochloride are suspended in 525 ml of isopropyl acetate, a solution of 104.8 g of potassium carbonate in 300 ml of water is added and then the mixture is stirred until the solid has disappeared. 77.4 g of acetic anhydride are added while maintaining the temperature below 20° C. and then the mixture is left stirring at 20° C. A precipitate is observed to form, which precipitate disappears when the mixture is heated at approximately 55-60° C. The organic phase is washed twice with 200 ml of water and is then cooled at 0-5° C. overnight. The product formed is recovered by filtration and is then washed twice with 100 ml of MTBE.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature below 20° C.
  2. waitthe mixture is left
  3. stirringstirring at 20° C
  4. customto form
  5. customwhich precipitate
  6. washThe organic phase is washed twice with 200 ml of water
  7. temperatureis then cooled at 0-5° C. overnight
  8. customThe product formed
  9. filtrationis recovered by filtration
  10. washis then washed twice with 100 ml of MTBE