HRID55318

反应详情

EQUATION

反应方程式

HRID 55318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 4-(2-t-butyldimethylsiloxyethyl)bromobenzene (1.00 g), methyl acrylate (0.55 g), palladium(II) acetate (0.010 g), triphenylphosphine (0.017 g) and N,N,N',N'-tetramethylethylenediamine (0.48 ml) was heated at 140° C. for 24 hours under an atmosphere of argon. To the reaction mixture was added methylene chloride (30 ml), the formed insoluble materials were removed by filtration through a celite column, and the filtrate was concentrated under reduced pressure. To the residue was added diethyl ether (30 ml), and the formed insoluble materials were removed by filtration through a celite column. The filtrate was concentrated to dryness to give methyl 4-(2-t-butyldimethylsiloxyethyl)cinnamate (0.94 g) as a brown oily liquid.

WORKUP

后处理

  1. customthe formed insoluble materials were removed by filtration through a celite column
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the residue was added diethyl ether (30 ml)
  4. customthe formed insoluble materials were removed by filtration through a celite column
  5. concentrationThe filtrate was concentrated to dryness