HRID1712371

反应详情

EQUATION

反应方程式

HRID 1712371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The mixture of 2.50 g of 2-methoxy-6-methylphenol, 3.75 g of potassium carbonate and 18.3 ml of 1,3-dibromopropane in 50 ml of acetonitrile is stirred at reflux with stirring over 16 hours. The reaction mixture is cooled, diluted with 200 ml of water and extracted with tert-butyl methyl ether (2×200 ml). The organic phases are washed successively with water (200 ml) and brine (200 ml), dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained as a yellowish oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.59 (1:1 EtOAc-heptane); Rt=5.10.

WORKUP

后处理

  1. temperatureat reflux
  2. stirringwith stirring over 16 hours
  3. temperatureThe reaction mixture is cooled
  4. extractionextracted with tert-butyl methyl ether (2×200 ml)
  5. washThe organic phases are washed successively with water (200 ml) and brine (200 ml)
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated by evaporation