HRID363062

反应详情

EQUATION

反应方程式

HRID 363062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a reaction vessel were placed 0.26 g of zinc dust, 1.0 g of triphenylphosphine, 1.3 g of carbon tetrabromide and 20 ml of methylene chloride, followed by stirring at room temperature. After 24 hours, a solution of 0.70 g of (4-(2-chlorobenzyloxy)-3,5-dichlorophenoxy)acetaldehyde dissolved in 5 ml of methylene chloride was added dropwise to the above solution, while stirring at room temperature. After stirring at room temperature for 6 hours, the reaction mixture was concentrated to obtain a residue. The residue was subjected to silica gel chromatography, which afforded 0.63 g of 4-(2-chlorobenzyloxy)-3,5-dichloro-1-(3,3-dibromo-2-propenyloxy)benzene (63% yield), m.p. 83.5° C.

WORKUP

后处理

  1. customIn a reaction vessel were placed
  2. additionwas added dropwise to the above solution
  3. stirringwhile stirring at room temperature
  4. stirringAfter stirring at room temperature for 6 hours
  5. concentrationthe reaction mixture was concentrated
  6. customto obtain a residue