HRID414230

反应详情

EQUATION

反应方程式

HRID 414230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.82 g (50 mmol) of 1-(3-chlorophenyl)-2-phenyl-3-oxo-1-butene in 80 ml of ethanol are heated to reflux with 11.5 g (100 mmol) of methyl β-aminocrotonate and 6 ml (100 mmol) of acetic acid overnight. 11.5 g of methyl β-aminocrotonate and 6 ml of acetic acid are added once more, and the mixture is heated under reflux for 24 hours. On cooling, crystals are produced, and these are filtered off with suction and washed with ethanol. For complete purification, they are passed through a silica gel column using toluene/ethyl acetate 20:1. 5.3 g of a colorless substance, of melting point 191° C., are obtained.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 24 hours
  3. temperatureOn cooling
  4. customcrystals are produced
  5. filtrationthese are filtered off with suction
  6. washwashed with ethanol
  7. customFor complete purification, they
  8. custom5.3 g of a colorless substance, of melting point 191° C., are obtained