HRID2091390

反应详情

EQUATION

反应方程式

HRID 2091390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution (200 mL) of 1-(5-bromo-2-hydroxyphenyl)ethanone (25.0 g) in N,N-dimethylformamide were added potassium carbonate (24.0 g) and methyl bromoacetate (11.5 mL) at room temperature, and the mixture was stirred at room temperature for 15 hr. The reaction mixture was filtered, 1,8-diazabicyclo[5.4.0]undec-7-ene (23.2 mL) was added to the filtrate, and the mixture was stirred at 100° C. for 3 hr. The reaction mixture was allowed to cool to room temperature, and ice water was added. The precipitate was washed with ethanol-water to give the title object compound (16.8 g, 52%) as a pale-red solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. addition1,8-diazabicyclo[5.4.0]undec-7-ene (23.2 mL) was added to the filtrate
  3. stirringthe mixture was stirred at 100° C. for 3 hr
  4. temperatureto cool to room temperature
  5. additionice water was added
  6. washThe precipitate was washed with ethanol-water