HRID1089166

反应详情

EQUATION

反应方程式

HRID 1089166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

105.2 g of dichloromethoxymethane are added to a solution of 122.6 g of 1,2-dichloro-3,4-dimethoxybenzene in methylene chloride, and titanium tetrabromide is added dropwise to the mixture at -50° to -60° C. The mixture is stirred at room temperature for 20 hours. The reaction mixture is poured into water and the organic layer is separated. The aqueous layer is extracted with chloroform, and the extract and the above-obtained organic layer are combined. The mixture is washed with water, dried and evaporated to remove solvent. The residue is washed with n-hexane to give 106 g of 2,3-dichloro-4,5-dimethoxybenzaldehyde.

WORKUP

后处理

  1. additionis added dropwise to the mixture at -50° to -60° C
  2. customthe organic layer is separated
  3. extractionThe aqueous layer is extracted with chloroform
  4. extractionthe extract
  5. washThe mixture is washed with water
  6. customdried
  7. customevaporated
  8. customto remove solvent
  9. washThe residue is washed with n-hexane