HRID1386061

反应详情

EQUATION

反应方程式

HRID 1386061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8-amino-6-bromo-2,3-dimethylimidazo[1,2-a]pyridine (1.2 g, 5.0 mmol), 2,6-dimethylbenzylchloride (0.772 g, 5.0 mmol), sodium carbonate (0.8 g), sodium iodide (0.2 g) and acetone (45 ml) was stirred overnight. More 2,3-dimethylbenzylchloride (0.285 g) was added and the reaction mixture was refluxed for 5 h. After addition of acetone the reaction mixture was filtered. The solvent was removed in vacuo and the residue was dissolved in CH2Cl2, washed with NaHCO3, dried over Na2SO4 and evaporated. The crude product dissolved in ethyl acetate and petroleum ether was added. Filtration and evaporation of the solvent gave a residue which was recrystallized from ethyl acetate to give 1.45 g of the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 5 h
  2. filtrationwas filtered
  3. customThe solvent was removed in vacuo
  4. dissolutionthe residue was dissolved in CH2Cl2
  5. washwashed with NaHCO3
  6. dry with materialdried over Na2SO4
  7. customevaporated
  8. dissolutionThe crude product dissolved in ethyl acetate
  9. additionpetroleum ether was added
  10. filtrationFiltration and evaporation of the solvent
  11. customgave a residue which
  12. customwas recrystallized from ethyl acetate