HRID2254421

反应详情

EQUATION

反应方程式

HRID 2254421 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

54 mg of 4-fluoro-3-hydroxybenzaldehyde was dissolved in 2 ml of 2-propanol, and 73 mg of benzyl chloride, 80 mg of potassium carbonate and 5 mg of sodium iodide were added to the solution. The mixture was heated under reflux for 7 hours with stirring. The reaction mixture was diluted with ethyl ether, and the inorganic salts were removed by filtration. The filtrate was evaporated under reduced pressure, and purified by silica gel column chromatography (Wakogel C-200, 5 g; eluting solvent: hexane/ethyl acetate=20/1), and then recrystallized from chloroform/hexane to give 77 mg of 3-benzyloxy-4-fluorobenzaldehyde as colorless needles having a melting point of 68° to 69° C.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 7 hours
  3. customthe inorganic salts were removed by filtration
  4. customThe filtrate was evaporated under reduced pressure
  5. custompurified by silica gel column chromatography (Wakogel C-200, 5 g; eluting solvent: hexane/ethyl acetate=20/1)
  6. customrecrystallized from chloroform/hexane