HRID2167117

反应详情

EQUATION

反应方程式

HRID 2167117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Potassium carbonate (1.12 g) was added to a solution of methyl 2,4-dihydroxybenzoate (454 mg) and 2-bromo-4,5-dimethoxybenzyl bromide (1.0 g) in dry acetone (80 ml). The reaction mixture was heated to reflux at 80° C. for 4 hours. The solvents were removed under vacuum and the residue was re-dissolved in DCM and washed with water (3×). The organic layer was passed through a hydrophobic frit and concentrated under vacuum. The crude residue was purified by chromatography on silica gel, eluting with petrol and increasing amounts of ethyl acetate.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. customThe solvents were removed under vacuum
  3. dissolutionthe residue was re-dissolved in DCM
  4. washwashed with water (3×)
  5. concentrationconcentrated under vacuum
  6. customThe crude residue was purified by chromatography on silica gel
  7. washeluting with petrol
  8. temperatureincreasing amounts of ethyl acetate