HRID1741839

反应详情

EQUATION

反应方程式

HRID 1741839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (4-bromo-2-fluorobenzyl)triphenylphosphonium bromide (3.82 g) and potassium t-butoxide (786 mg) was stirred at room temperature for 30 minutes. Then acetone (1.0 ml) was added and the reaction mixture was heated at reflux for 40 hours. The mixture was filtered, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, washed with water and brine, dried over magnesium sulfate and the solvent was evaporated. The residue was chromatographed on silica gel column eluting with hexane to give 1-(4-bromo-2-fluorophenyl)-2-methyl-1-propene (0.70 g) as an oil.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 40 hours
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washwashed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent was evaporated
  9. customThe residue was chromatographed on silica gel column
  10. washeluting with hexane