HRID2417397

反应详情

EQUATION

反应方程式

HRID 2417397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

To a mixture of 4-acetoxy-2-bromo-3-methoxybenzaldehyde (546 mg, 2 mmol; prepared in example 105, step a), 2-methoxy-phenol (280 mg, 2 mmol) and cesium carbonate (1.3 g, 4 mmol) in 16 mL of pyridine was added copper oxide(320 mg, 4 mmol)under argon. The mixture was purged with argon for 10 min, heated at 130° C. overnight and then quenched with 5% HCl solution. The mixture was extracted with ethyl acetate, washed with 1N NaOH solution and water before drying over sodium sulfate. After the removal of the solvent, the residue was chromatographed to give the product, 4-hydroxy-5-methoxy-2-(2-methoxy-phenoxy)-benzaldehyde.

WORKUP

后处理

  1. customThe mixture was purged with argon for 10 min
  2. customquenched with 5% HCl solution
  3. extractionThe mixture was extracted with ethyl acetate
  4. washwashed with 1N NaOH solution and water
  5. dry with materialbefore drying over sodium sulfate
  6. customAfter the removal of the solvent
  7. customthe residue was chromatographed