反应详情

A solution of 2,3-diamino-5-methyl-pyridine (2.3 g, 19 mmol) and 3-bromo-2-oxo-butyric acid ethyl ester (4.3 g, 21 mmol) in ethanol (25 ml) was refluxed for 20 h. Sodium carbonate (2.6 g, 25 mmol) was added and the mixture was filtrated and the solids were washed with ethanol. The filtrate and washings were combined and evaporated under reduced pressure. The residue was dissolved in methylene chloride, washed twice with a sodium carbonate solution and twice 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 (9:1) as eluent gave 1.3 g (30%) of the title compound as an oil.

1. filtrationthe mixture was filtrated
2. washthe solids were washed with ethanol
3. customevaporated under reduced pressure
4. dissolutionThe residue was dissolved in methylene chloride
5. washwashed twice with a sodium carbonate solution and twice with water
6. customThe organic layer was separated
7. dry with materialdried (Na2SO4)
8. customevaporated under reduced pressure
9. customPurification of the residue by column chromatography on silica gel