HRID5429

反应详情

EQUATION

反应方程式

HRID 5429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of cysteamine hydrochloride (2.95 g, 26 mmoles) in ethanol (100 ml) was added 60% sodium hydride (oily; 2.08 g, 26 mmoles) with stirring under ice-cooling and the mixture was stirred for 5 minutes. 5-chloro-2-methylimidazo[1,2-a]pyridine (3.33 g, 20 mmoles) was added to the mixture, followed by heating at reflux for 3 hours. After the solvent was distilled off, chloroform was added to the residue which was washed with 1N-NaOH and dried over anhydrous potassium carbonate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate/ethanol/triethylamine=6:2:1) to obtain 2.2 g of the desired product (53.6%, brown oily product).

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture was stirred for 5 minutes
  3. temperatureby heating
  4. temperatureat reflux for 3 hours
  5. distillationAfter the solvent was distilled off
  6. additionchloroform was added to the residue which
  7. washwas washed with 1N-NaOH
  8. dry with materialdried over anhydrous potassium carbonate
  9. distillationAfter the solvent was distilled off
  10. customthe residue was purified by column chromatography (eluent: ethyl acetate/ethanol/triethylamine=6:2:1)