HRID2073924

反应详情

EQUATION

反应方程式

HRID 2073924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-Chloro-3',4'-dimethoxy benzophenone (6.29 g, 25 mmol), sodium tert.-amylate (5.50 g, 50 mmol), acetyl morpholine (23.90 g, 185 mmol), and anhydrous toluene (50 ml) were stirred under reflux for 8 hours. After cooling, the solution was washed twice with water, dried, and the toluene distilled off on a rotary evaporator. The viscous residue was stirred at 50° C. with diisopropyl ether (40 ml), whereupon the substance solidified. After it had cooled to room temperature, the crude product was crushed, filtered by suction, washed with diisopropyl ether (2×5 ml) and dried.

WORKUP

后处理

  1. temperatureunder reflux for 8 hours
  2. temperatureAfter cooling
  3. washthe solution was washed twice with water
  4. customdried
  5. distillationthe toluene distilled off on a rotary evaporator
  6. temperatureAfter it had cooled to room temperature
  7. customthe crude product was crushed
  8. filtrationfiltered by suction
  9. washwashed with diisopropyl ether (2×5 ml)
  10. customdried