HRID5472

反应详情

EQUATION

反应方程式

HRID 5472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-mercaptoimidazo[1,2-a]pyridine (1.50 g, 10 mmoles) and 4M sodium methylate (2.93 ml, 12 mmoles) in ethanol (50 ml) was added 3-methylsulfonylamino-1-methylsulfonyloxypropane (2.77 g, 12 mmoles) at room temperature and the mixture was heated under reflux for 16 hours. After cooling, the solvent was distilled off. The residue was dissolved in chloroform, washed with an aqueous saturated sodium bicarbonate solution and dried. After the solvent was distilled off, the residue was purified by column chromatography [eluent: ethyl acetate/ethanol (50:1)] to obtain 1.34 g of the desired product (47.5%, pale yellow crystals).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 hours
  3. temperatureAfter cooling
  4. distillationthe solvent was distilled off
  5. dissolutionThe residue was dissolved in chloroform
  6. washwashed with an aqueous saturated sodium bicarbonate solution
  7. customdried
  8. distillationAfter the solvent was distilled off
  9. customthe residue was purified by column chromatography [eluent: ethyl acetate/ethanol (50:1)]