HRID1816686

反应详情

EQUATION

反应方程式

HRID 1816686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 1-bromo-4-(6-bromohexyloxy)benzene (6.0 g) and sodium methylate (28% in methanol) (10.3 ml) in methanol (30 ml) was stirred for 2 hours at 70° C. (bath temp.), and then the solvent was evaporated. The residue was neutralized by 1N-hydrochloric acid and extracted with ethyl acetate (100 ml), and washed with water and brine. The organic layer was dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give a crude product. The crude product was purified by silica gel chromatography (20:1-10:1 hexane-ethyl acetate) to give 1-bromo-4-(6-methoxyhexyloxy)benzene (15.61 g) as a colorless oil.

WORKUP

后处理

  1. customthe solvent was evaporated
  2. extractionextracted with ethyl acetate (100 ml)
  3. washwashed with water and brine
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationMagnesium sulfate was filtered off
  6. customthe filtrate was evaporated under reduced pressure
  7. customto give a crude product
  8. customThe crude product was purified by silica gel chromatography (20:1-10:1 hexane-ethyl acetate)