HRID1194365

反应详情

EQUATION

反应方程式

HRID 1194365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

24.1 g (0.098 mole) of 2-bromo-3-methoxy-6-methoxymethylphenol and 27.7 g of methyl iodide are dissolved in 200 ml of acetone in the presence of 14.82 g (0.107 mole) of potassium carbonate. This solution is heated at reflux temperature, with stirring, for 2.5 hours. It is then cooled, the mineral salts are filtered off and the filtrate is distilled to remove the acetone. The residue is taken up in water and extracted with dichloromethane. The organic phase is dried over anhydrous sodium sulfate and distilled under reduced pressure. 13.1 g of 1-bromo-2,6-dimethoxy-3-methoxymethylbenzene are obtained. Yield: 51% of theory; B.P.: 92°-115° C./0.005 mbar.

WORKUP

后处理

  1. temperatureThis solution is heated
  2. temperatureat reflux temperature
  3. temperatureIt is then cooled
  4. filtrationthe mineral salts are filtered off
  5. distillationthe filtrate is distilled
  6. customto remove the acetone
  7. extractionextracted with dichloromethane
  8. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  9. distillationdistilled under reduced pressure