HRID12293

反应详情

EQUATION

反应方程式

HRID 12293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 g of 5-bromo-2-hydroxy-3-methoxybenzaldehyde, 23.9 g of potassium carbonate and 12.2 g of (2-chloromethoxyethyl)trimethylsilane is suspended in 500 ml of DMF and stirred at room temperature for 48 hours. The DMF is distilled off in vacuo, the residue is dissolved in ethyl acetate, and the resulting solution is extracted with water. It is then dried over magnesium sulphate and filtered, and the solvent is distilled off. The crude product is purified by silica gel chromatography (heptane/ethyl acetate).

WORKUP

后处理

  1. distillationThe DMF is distilled off in vacuo
  2. dissolutionthe residue is dissolved in ethyl acetate
  3. extractionthe resulting solution is extracted with water
  4. dry with materialIt is then dried over magnesium sulphate
  5. filtrationfiltered
  6. distillationthe solvent is distilled off
  7. customThe crude product is purified by silica gel chromatography (heptane/ethyl acetate)