HRID1068817

反应详情

EQUATION

反应方程式

HRID 1068817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.07 g (17.1 mmol) of 5-chloro-3-ethoxycarbonyl-2-methylimidazo[1,2-a]pyridine, 3.48 g (25.6 mmol) of 2-(4-aminophenyl)ethylamine and 4.41 g (34.1 mmol) of N,N-diisopropylethylamine in 60 ml of acetonitrile was heated for 64 hours under reflux with stirring. After cooling, the solvent was distilled off. To the residue was added chloroform. The residue was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off. The residue was purified by column chromatography (eluent: chloroform/methanol=30:1) and recrystallized from ethyl acetate-n-hexane to give 4.37 g of the desired compound (75.7%, pale brown crystals).

WORKUP

后处理

  1. temperaturewas heated for 64 hours
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. distillationthe solvent was distilled off
  5. additionTo the residue was added chloroform
  6. washThe residue was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off
  9. customThe residue was purified by column chromatography (eluent: chloroform/methanol=30:1)
  10. customrecrystallized from ethyl acetate-n-hexane