反应详情

Ethyl 8-amino-3-methylimidazo[1,2-a]pyridine-2-carboxylate (4.6 g, 21 mmol), 2,6-dimethylbenzyl chloride (3.2 g, 21 mmol), sodium carbonate (4.4 g, 42 mmol) and a cat. amount of potassium iodide were added to acetonitrile (50 ml) and refluxed for 3 h., stirred for 20 h. at room temperature and refluxed for 1 h. The solids were removed by filtration and the solvents were evaporated under reduced pressure. The residue was dissolved in methylene chloride and washed with water. The organic layer was separated, dried (Na2SO4) and evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using methylene chloride:methanol (10:1) as eluent and crystallization from ethyl acetate gave 4.0 g (56%) of the desired product.

1. temperaturerefluxed for 3 h.
2. temperaturerefluxed for 1 h
3. customThe solids were removed by filtration
4. customthe solvents were evaporated under reduced pressure
5. dissolutionThe residue was dissolved in methylene chloride
6. washwashed with water
7. customThe organic layer was separated
8. dry with materialdried (Na2SO4)
9. customevaporated under reduced pressure
10. customPurification of the residue by column chromatography on silica gel
11. customcrystallization from ethyl acetate