HRID37841

反应详情

EQUATION

反应方程式

HRID 37841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of p-nitro-phenol (6.0 g, 43.1 mmol), potassium carbonate (14.9 g, 108 mmol) and 1,2-dibromoethane (24.3 g, 129 mmol) in butanone (80 mL) was heated at reflux for 18 h. The mixture was cooled, the inorganic salts filtered and the filtrate concentrated under vacuum to give a brown viscous liquid, which was partitioned between dichloromethane and water. The organic phase was separated and concentrated in vacuo to obtain a residue which was purified by column chromatography using 4% ethyl acetate in petroleum ether as eluent to afford 1-(2-bromo-ethoxy)-4-nitro-benzene (7.5 g, 70%) as a light yellow solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 18 h
  3. temperatureThe mixture was cooled
  4. filtrationthe inorganic salts filtered
  5. concentrationthe filtrate concentrated under vacuum
  6. customto give a brown viscous liquid, which
  7. customwas partitioned between dichloromethane and water
  8. customThe organic phase was separated
  9. concentrationconcentrated in vacuo
  10. customto obtain a residue which
  11. customwas purified by column chromatography