HRID231530

反应详情

EQUATION

反应方程式

HRID 231530 的结构方程式

PROCEDURE

实验过程

A mixture of 50.0 g of 3,4-dichloroacetophenone and 75 ml of N,N-dimethylformamide dimethyl acetal was heated under reflux for 6 hours, then allowed to cool for 16 hours. The crystalline precipitate was collected by filtration, washed with hexane and dried. The addition of hexane to the above filtrate precipitated some additional product which was collected by filtration. The precipitates were combined, washed with hexane and dried in vacuo to give 55.0 g of 3',4'-dichloro-3-dimethylaminoacrylophenone as bright yellow crystals.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. temperatureto cool for 16 hours
  4. filtrationThe crystalline precipitate was collected by filtration
  5. washwashed with hexane
  6. customdried
  7. additionThe addition of hexane to the above filtrate
  8. customprecipitated some additional product which
  9. filtrationwas collected by filtration
  10. washwashed with hexane
  11. customdried in vacuo