HRID2383368

反应详情

EQUATION

反应方程式

HRID 2383368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 2-(4-bromophenyl)ethanol (48.3 g) in acetonitrile (480 mL) was added diisopropylethylamine (46.6 g), N-vinylphthalimide (43.7 g) and tri-o-tolylphosphine (7.31 g) and the mixture was purged with nitrogen gas three times. Palladium acetate (2.7 g) was added and the mixture was stirred at 90° C. for 21 hr under nitrogen. The reaction was cooled and the precipitated product collected by filtration. The resulting solid was re-dissolved in dichloromethane and ethyl acetate and filtered through silica gel. The filtrate was concentrated in vacuo to give the title compound, 24 g.

WORKUP

后处理

  1. customthe mixture was purged with nitrogen gas three times
  2. additionPalladium acetate (2.7 g) was added
  3. temperatureThe reaction was cooled
  4. filtrationthe precipitated product collected by filtration
  5. dissolutionThe resulting solid was re-dissolved in dichloromethane
  6. filtrationethyl acetate and filtered through silica gel
  7. concentrationThe filtrate was concentrated in vacuo