HRID1395087

反应详情

EQUATION

反应方程式

HRID 1395087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

1290 g of aluminium chloride (9.6 mole) were suspended with stirring in 1500 ml of carbon disulphide. 405 g of acetanilide (3 moles) were added slowly to this suspension, while the temperature was kept at 25° C. The reaction mixture was heated until reflux and was cooled immediately to 25° C. 565 ml of propionyl chloride (6.5 moles) were added dropwise in such a way that the temperature was kept at 25° C. The reaction mixture was heated until reflux for 5 hours and kept overnight at ambient temperature (20° C.). The supernatant carbon disulphide layer was decanted and the remaining viscous mixture was poured in a mixture of ice and hydrochloric acid. The residue formed was filtered off and further recrystallized from a mixture of 1500 ml of ethanol and 75 ml of water. Drying was applied under vacuum at 100° C. A light yellow powder was obtained.

WORKUP

后处理

  1. customwas kept at 25° C
  2. temperatureThe reaction mixture was heated
  3. temperatureuntil reflux
  4. customwas kept at 25° C
  5. temperatureThe reaction mixture was heated
  6. temperatureuntil reflux for 5 hours
  7. custom(20° C.)
  8. customThe supernatant carbon disulphide layer was decanted
  9. additionthe remaining viscous mixture was poured in a mixture of ice and hydrochloric acid
  10. customThe residue formed
  11. filtrationwas filtered off
  12. customfurther recrystallized from a mixture of 1500 ml of ethanol and 75 ml of water
  13. customDrying
  14. customwas applied under vacuum at 100° C
  15. customA light yellow powder was obtained