HRID618003

反应详情

EQUATION

反应方程式

HRID 618003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of 2.76 g (0.115 mol) of magnesium in 75 mL of diethylether, was slowly added 24.31 g (0.143 mol) isopropyl iodide. The resulting reaction mixture was allowed to react until all of the magnesium was consumed. Then, a solution of 15.0 g (0.92 mol) of 2,3-dimethoxy benzonitrile in 75 mL of diethylether was added over ninety minutes. The resulting reaction mixture was reacted overnight at room temperature and then refluxed for four hours. The resultant reaction mixture was then cooled to 0° C., and the top layer was decanted into saturated ammonium chloride and ice. The resultant layers were separated and the organic layer was washed sequentially with a dilute sodium hydroxide solution, water, and a dilute hydrochloric acid solution, dried over sodium sulfate, filtered and then concentrated to provide an orange oil. This oil was distilled under reduced pressure (5 inch vigreux column; 0.2 mm Hg) to provide 6.25 g of an orange oil.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. customwas consumed
  3. customThe resulting reaction mixture
  4. customwas reacted overnight at room temperature
  5. temperaturerefluxed for four hours
  6. customThe resultant reaction mixture
  7. customthe top layer was decanted into saturated ammonium chloride and ice
  8. customThe resultant layers were separated
  9. washthe organic layer was washed sequentially with a dilute sodium hydroxide solution, water
  10. dry with materiala dilute hydrochloric acid solution, dried over sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customto provide an orange oil
  14. distillationThis oil was distilled under reduced pressure (5 inch vigreux column; 0.2 mm Hg)