HRID974110

反应详情

EQUATION

反应方程式

HRID 974110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

136 ml of a 1.6M n-butyl lithium solution in hexane are added to a solution of 48.5 g of 3,4,5-trimethoxybenzaldehyde dimethyl acetal in 485 ml of benzene under stirring at 0° C. for about 20 minutes. The mixture is further stirred at 0° C. for 30 minutes, and 33.2 g of 3,4-dimethoxybenzaldehyde are added thereto. After stirring the mixture at 0° to 10° C. for 2 hours, 485 ml of water and 16 g of citric acid are added thereto. After shaking the mixture, the organic layer is separated therefrom, washed with water and evaporated under reduced pressure to remove solvent. 78.5 g of 2-(3,4-dimethoxy-α-hydroxybenzyl)-3,4,5-trimethoxybenzaldehyde dimethyl acetal are thereby obtained as a yellow oil.

WORKUP

后处理

  1. stirringThe mixture is further stirred at 0° C. for 30 minutes
  2. stirringAfter stirring the mixture at 0° to 10° C. for 2 hours
  3. stirringAfter shaking the mixture
  4. customthe organic layer is separated
  5. washwashed with water
  6. customevaporated under reduced pressure
  7. customto remove solvent