HRID1089169

反应详情

EQUATION

反应方程式

HRID 1089169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.51 g of boron tribromide in methylene chloride is added to dropwise to a solution of 0.47 g of 2,3-dichloro-4,5-dimethoxybenzaldehyde in methylene chloride at -50° to -60° C. and the mixture is stirred at -50° C. to room temperature for 1 hour. The reaction mixture is poured into water and the aqueous mixture is extracted with ethyl acetate. The extract is evaporated to remove solvent. Methanol and 10% hydrochloric acid are added to the residue and the mixture is stirred at room temperature for 1 hour. To the reaction mixture are added water, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is washed with n-hexane and dried to give 0.38 g of 2,3-dichloro-4,5-dihydroxybenzaldehyde.

WORKUP

后处理

  1. extractionthe aqueous mixture is extracted with ethyl acetate
  2. customThe extract is evaporated
  3. customto remove solvent
  4. additionMethanol and 10% hydrochloric acid are added to the residue
  5. stirringthe mixture is stirred at room temperature for 1 hour
  6. additionTo the reaction mixture are added water
  7. extractionthe mixture is extracted with ethyl acetate
  8. washThe extract is washed with water
  9. customdried
  10. customevaporated
  11. customto remove solvent
  12. washThe residue is washed with n-hexane
  13. customdried