HRID1976208

反应详情

EQUATION

反应方程式

HRID 1976208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Toluene-4-sulfonic acid, 2-hydroxyphenyl ester (0.64 g, 2.42 mmol), 4-bromomethyl-1,3-dimethoxy-benzene (0.56 g, 2.42 mmol), potassium carbonate (0.36 g, 2.62 mmol) and 18-crown-6-ether (0.06 g, 0.24 mmol) were stirred together at room temperature in acetone (20 cm3, 99%) under nitrogen for 28 hours. The solution was evaporated under reduced pressure, and the residue was taken up in dichloromethane (20 cm3) and water (20 cm3). The aqueous layer was extracted with dichloromethane (2×20 cm3), and the combined extracts were washed with water (2×50 cm3), dried (MgSO4), and evaporated under reduced pressure. The residue was chromatographed (SiO2, dichloromethane) to give the ether, (0.84 g, 83%) as a clear oil.

WORKUP

后处理

  1. customThe solution was evaporated under reduced pressure
  2. extractionThe aqueous layer was extracted with dichloromethane (2×20 cm3)
  3. washthe combined extracts were washed with water (2×50 cm3)
  4. dry with materialdried (MgSO4)
  5. customevaporated under reduced pressure
  6. customThe residue was chromatographed (SiO2, dichloromethane)
  7. customto give the ether, (0.84 g, 83%) as a clear oil