HRID1489185

反应详情

EQUATION

反应方程式

HRID 1489185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Triethylamine (219 ml) was added to a solution of 4-bromophenol (259 g) and 4-dimethylaminopyridine (1.5 g) in dichloromethane (1000 ml) at 0° C. at such a rate that the temperature did not rise above 20° C. When the addition was complete propionyl chloride (137 ml) was added in portions over 1 hour such that the temperature did not rise above 20° C. Finally, the mixture was stirred at room temperature for 2 hours. Water (700 ml) was added and the layers were separated. The dichloromethane solution was washed with brine (500 ml), dried (MgSO4) and concentrated in vacuo to give the title compound as an oil, 344 g.

WORKUP

后处理

  1. customdid not rise above 20° C
  2. additionWhen the addition
  3. additionwas added in portions over 1 hour such that the temperature
  4. customdid not rise above 20° C
  5. customthe layers were separated
  6. washThe dichloromethane solution was washed with brine (500 ml)
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo