HRID537678

反应详情

EQUATION

反应方程式

HRID 537678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(5-bromo-2-ethylphenyl)-2,2,6,6-tetramethylpyran-3,5-dione (200 mg, 0.57 mmol), 4-chlorophenol (110 mg, 0.86 mmol), copper(I) iodide (109 mg, 0.57 mmol), 1,10-phenanthroline (103 mg, 0.57 mmol) and potassium phosphate (483 mg, 2.28 mmol), in dimethylsulfoxide (3.5 ml) is heated to 200° C. under microwave irradiation for 30 minutes. The mixture is cooled to room temperature, poured into 2M aqueous hydrochloric acid and extracted with dichloromethane. The organic extract is washed with water, dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure. The solvent is evaporated under reduced pressure and the residue is purified by column chromatography on silica gel to give 4-[5-(4-chlorophenoxy)-2-ethylphenyl]-2,2,6,6-tetramethylpyran-3,5-dione.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. extractionThe organic extract
  3. washis washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate is evaporated under reduced pressure
  7. customThe solvent is evaporated under reduced pressure
  8. customthe residue is purified by column chromatography on silica gel