HRID454789

反应详情

EQUATION

反应方程式

HRID 454789 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-bromo-2′,4′-dimethoxyacetophenone (5 g, 19.1 mmols) in 25 mL of 2-butanone was added to a suspension of phenol (1.8 g, 19.1 mmols), K2CO3 (2.6 g, 19.1 mmols) and KI (41.5 mg, 0.25 mmols) in 20.0 mL of the same solvent. The solution was then refluxed for 20 hours. The mixture was filtered and the solvent was evaporated off under vacuum. The residue obtained was dissolved in EtOAc and washed with a 10% aqueous solution of NaOH and then with water. The organic extract was dried over Na2SO4, filtered and evaporated under vacuum. Finally, the crude residue was washed with Et2O and dried under low pressure to provide 4.4 g (yield: 84%) of the title compound.

WORKUP

后处理

  1. temperatureThe solution was then refluxed for 20 hours
  2. filtrationThe mixture was filtered
  3. customthe solvent was evaporated off under vacuum
  4. customThe residue obtained
  5. washwashed with a 10% aqueous solution of NaOH
  6. extractionThe organic extract
  7. dry with materialwas dried over Na2SO4
  8. filtrationfiltered
  9. customevaporated under vacuum
  10. washFinally, the crude residue was washed with Et2O
  11. customdried under low pressure