反应详情

To a suspension of 5-mercaptoimidazo[1,2-a]pyridine (1.50 g, 10 moles) in ethanol (100 ml) was added a solution of 4.1M sodium methylate (2.44 ml, 10 mmoles) in methanol and the mixture was stirred at room temperature for 10 minutes. To the reaction mixture was added 1-methylsulfonyl-4-methylsulfonyloxypiperidine (2.83 g, 11 mmoles) at room temperature and the mixture was heated under reflux for 14 hours. After the solvent was distilled off, the residue was dissolved in chloroform, which was washed in turn with an aqueous 1N sodium hydroxide solution and water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography [eluent:ethyl acetate/ethanol (10:1)] to obtain 1.27 g of the desired product (40.8%, light brown solid).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 14 hours
3. distillationAfter the solvent was distilled off
4. dissolutionthe residue was dissolved in chloroform
5. washwhich was washed in turn with an aqueous 1N sodium hydroxide solution and water
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationAfter the solvent was distilled off
8. customthe residue was purified by column chromatography [eluent:ethyl acetate/ethanol (10:1)]